Composition and method for treating plants with exogenous chemicals

ABSTRACT

A composition is disclosed for application to a plant that comprises an exogenous chemical (for example, a postemergent herbicide), an aqueous diluent, and a first excipient substance that is amphiphilic. The weight/weight ratio of the first excipient substance to the exogenous chemical is between about 1:3 and about 1:100. The aqueous composition forms anisotropic aggregates on a wax layer, and the presence of the anisotropic aggregates can be detected by a test described herein. Compositions of the present invention, when applied to plants, provide enhanced biological activity per unit amount of exogenous chemical, as compared to otherwise similar compositions containing surfactants that do not form anisotropic aggregates. Without being bound by theory, it is presently believed that this enhanced biological activity results from the formation or enlargement of hydrophilic channels through the epicuticular wax of the plant.

This application claims the benefit of provisional application Ser. No. 60/029,317, filed Oct. 25, 1996; provisional application Ser. No. 60/034,887, filed Jan. 31, 1997; and provisional application Ser. No. 60/039,789, filed Mar. 4, 1997. Each of those provisional applications is incorporated here by reference.

BACKGROUND OF THE INVENTION

This invention relates to formulations and methods for enhancing the efficacy of exogenous chemicals used in treating plants. An exogenous chemical, as defined herein, is any chemical substance, whether naturally or synthetically derived, which (a) has biological activity or is capable of releasing in a plant an ion, moiety or derivative which has biological activity, and (b) is applied to a plant with the intent or result that the chemical substance or its biologically active ion, moiety or derivative enter living cells or tissues of the plant and elicit a stimulatory, inhibitory, regulatory, therapeutic, toxic or lethal response in the plant itself or in a pathogen, parasite or feeding organism present in or on the plant. Examples of exogenous chemical substances include, but are not limited to, chemical pesticides (such as herbicides, algicides, fungicides, bactericides, viricides, insecticides, aphicides, miticides, nematicides, molluscicides, and the like), plant growth regulators, fertilizers and nutrients, gametocides, defoliants, desiccants, mixtures thereof, and the like.

Exogenous chemicals, including foliar-applied herbicides, have at times been formulated with surfactants, so that when water is added, the resulting sprayable composition is more easily and effectively retained on the foliage (e.g., the leaves or other photosynthesizing organs) of plants. Surfactants can also bring other benefits, including improved contact of spray droplets with a waxy leaf surface and, in some cases, improved penetration of the accompanying exogenous chemical into the interior of leaves. Through these and perhaps other effects, surfactants have long been known to increase the biological effectiveness of herbicide compositions, or other compositions of exogenous chemicals, when added to or included in such compositions. Thus, for example, the herbicide glyphosate (N-phosphonomethylglycine) has been formulated with surfactants such as polyoxyalkylene-type surfactants including, among other surfactants, polyoxyalkylene alkylamines. Commercial formulations of glyphosate herbicide marketed under the trademark ROUNDUP® have been formulated with a surfactant composition based on such a polyoxyalkylene alkylamine, in particular a polyethoxylated tallowamine, this surfactant composition being identified as MON 0818. Surfactants have generally been combined with glyphosate or other exogenous chemicals either in a commercial concentrate (herein referred to as a "coformulation"), or in a diluted mixture that is prepared from separate compositions, one comprising an exogenous chemical (e.g. glyphosate) and another comprising surfactant, prior to use in the field (i.e., a tank mix).

Various combinations of exogenous chemicals and surfactants or other adjuvants have been tested in the past. In some instances, the addition of a particular surfactant has not produced uniformly positive or negative changes in the effect of the exogenous chemical on the plant (e.g., a surfactant that may enhance the activity of a particular herbicide on certain weeds may interfere with, or antagonize, the herbicidal efficacy on another weed species).

Some surfactants tend to degrade fairly rapidly in aqueous solutions. As a result, surfactants that exhibit this property can only be used effectively in tank mixes (i.e., mixed with the other ingredients in solution or dispersion in the tank soon before spraying is to occur), rather than being coformulated in an aqueous composition with the other ingredients in the first instance. This lack of stability, or inadequate shelf-life, has hindered the use of certain surfactants in some exogenous chemical formulations.

Other surfactants, though chemically stable, are physically incompatible with certain exogenous chemicals, particularly in concentrate coformulations. For example, most classes of nonionic surfactant, including polyoxyethylene alkylether surfactants, do not tolerate solutions of high ionic strength, as for example in a concentrated aqueous solution of a salt of glyphosate. Physical incompatibility can also lead to inadequate shelf-life. Other problems that can arise from such incompatibility include the formation of aggregates large enough to interfere with commercial handling and application, for example by blocking spray nozzles.

Another problem that has been observed in the past is the effect of environmental conditions on uptake of an exogenous chemical composition into foliage of a plant. For example, conditions such as temperature, relative humidity, presence or absence of sunlight, and health of the plant to be treated, can affect the uptake of a herbicide into the plant. As a result, spraying exactly the same herbicidal composition in two different situations can result in different herbicidal control of the sprayed plants.

One consequence of the above-described variability is that often a higher rate of herbicide per unit area is applied than might actually be required in that situation, in order to be certain that adequate control of undesired plants will be achieved. For similar reasons, other foliar-applied exogenous chemicals are also typically applied at significantly higher rates than needed to give the desired biological effect in the particular situation where they are used, to allow for the natural variability that exists in efficiency of foliar uptake. A need therefore exists for compositions of exogenous chemicals that, through more efficient uptake into plant foliage, allow reduced use rates.

Many exogenous chemicals are commercially packaged as a liquid concentrate that contains a significant amount of water. The packaged concentrate is shipped to distributors or retailers. Ultimately the packaged concentrate ends up in the hands of an end user, who further dilutes the concentrate by adding water in accordance with label instructions on the package. The dilute composition thus prepared is then sprayed on plants.

A significant portion of the cost of such packaged concentrates is the cost of transporting the concentrate from the manufacturing site to the location where the end user purchases it. Any liquid concentrate formulation that contained relatively less water and thus more exogenous chemical would reduce the cost per unit amount of exogenous chemical. However, one important limit on the ability of the manufacturer to increase the loading of the exogenous chemical in the concentrate is the stability of that formulation. With some combinations of ingredients, a limit will be reached at which any further reduction of water content in the concentrate will cause it to become unstable (e.g., to separate into discrete layers), which may make it commercially unacceptable.

Accordingly, a need exists for improved formulations of exogenous chemicals, particularly herbicides, that are stable, effective, less sensitive to environmental conditions, and permit the use of reduced amounts of exogenous chemical to achieve the desired biological effect in or on plants. A need also exists for stable liquid concentrate formulations of exogenous chemicals that contain less water and more exogenous chemical than prior art concentrates.

SUMMARY OF THE INVENTION

The present invention relates to novel methods and compositions wherein exogenous chemicals are applied to plants to generate a desired biological response.

One embodiment of the present invention is a method of applying an exogenous chemical to a plant, comprising the steps of (a) contacting foliage of the plant with a biologically effective amount of the exogenous chemical, and (b) contacting the same foliage with an aqueous composition that comprises a first excipient substance that is amphiphilic. The weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100. Further, the aqueous composition forms anisotropic aggregates in or on a wax layer as explained below. "Contacting" in this context means placing the substance or composition on the foliage. "Amphiphilic" means having at least one polar, water-soluble head group which is hydrophilic and at least one water-insoluble organic tail which is hydrophobic, contained within the same molecule.

In this method, step (b) can occur simultaneously with or within about 96 hours before or after step (a). In embodiments of the method in which the two steps occur simultaneously, either the exogenous chemical and the aqueous composition can be applied to the plant separately, for example by two spray nozzles directed at the same foliage, or the exogenous chemical can be contained within the aqueous composition, for example in a tank mix or coformulation.

Formation of anisotropic aggregates in or on a wax layer is determined by a test described in detail subsequently herein. In general, the test, as it applies to a composition comprising an exogenous chemical, comprises the steps of (1) providing a glass microscope slide coated with a thin, uniform layer of wax, such that the wax layer on the slide exhibits a dark field when illuminated by transmitted polarized light and examined through a microscope, (2) preparing a sample of an aqueous solution or dispersion of the composition to be tested, diluted or concentrated if necessary such that the concentration of exogenous chemical is about 15% to about 20% by weight of the composition, (3) positioning the wax-coated slide on the stage of a microscope that transmits polarized light through the slide, (4) placing a drop of the sample on the wax on the slide to form an assay slide, (5) maintaining the assay slide at approximately ambient temperature for a period of about 5 to about 20 minutes, and (6) determining, at the end of that period, whether when transmitting polarized light the locus of the drop on the slide displays birefringence. Birefringence at 5-20 minutes indicates the presence of anisotropic aggregates in or on the wax layer, while the absence of birefringence at that time indicates the absence of anisotropic aggregates as defined herein.

The test, as it applies to an aqueous composition of one or more excipient substances, not itself containing an exogenous chemical but intended for application to foliage of a plant in conjunction with an exogenous chemical, is as just described, except that in step (2) the composition is diluted or concentrated so that the concentration of the first excipient substance is approximately 5% to 7% by weight.

An "excipient substance" as that term is used in this patent is any substance other than an exogenous chemical and water that is added to the composition. "Excipient substances" include inert ingredients, although an excipient substance useful in the present invention does not have to be devoid of biological activity.

Another embodiment of the present invention is a plant treatment composition comprising (a) an exogenous chemical, and (b) a first excipient substance that is amphiphilic. As described above, the weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100, and in presence of water said composition forms anisotropic aggregates in or on a wax layer. This composition can be used in a method of treating plants, in which foliage of the plant is contacted with a biologically effective amount of a composition as described above and further comprising an aqueous diluent.

A wide variety of exogenous chemicals can be used in the compositions and methods of the present invention. A preferred class is foliar-applied exogenous chemicals, i.e. exogenous chemicals that are normally applied post-emergence to foliage of plants. A preferred subclass of foliar-applied exogenous chemicals is those that are water-soluble. By "water-soluble" in this context is meant having a solubility in distilled water at 25° C. greater than about 1% by weight. Especially preferred water-soluble exogenous chemicals are salts that have an anion portion and a cation portion. In one embodiment of the invention, at least one of the anion and cation portions is biologically active and has a molecular weight of less than about 300. Particular examples of such exogenous chemicals where the cation portion is biologically active are paraquat, diquat and chlormequat. More commonly it is the anion portion that is biologically active.

Another preferred subclass of exogenous chemicals is those that exhibit systemic biological activity in the plant. Within this subclass, an especially preferred group of exogenous chemicals is N-phosphonomethylglycine and its herbicidal derivatives. N-phosphonomethylglycine, often referred to by its common name glyphosate, can be used in its acid form, but is more preferably used in the form of a salt. Any water-soluble salt of glyphosate can be used in the practice of this invention. Some preferred salts include the sodium, potassium, ammonium, mono-, di-, tri- and tetra-C₁₋₄ -alkylammonium, mono-, di- and tri-C₁₋₄ -alkanolammonium, mono-, di- and tri-C₁₋₄ -alkylsulfonium and sulfoxonium salts. The ammonium, monoisopropylammonium and trimethylsulfonium salts of glyphosate are especially preferred. Mixtures of salts can also be useful in certain situations.

A composition of the present invention comprising an exogenous chemical and a first excipient substance as described above can have a number of different physical forms. For example, the composition can further comprise water in an amount effective to make the composition a dilute aqueous composition ready for application to foliage of a plant. Such a composition typically contains about 0.02 to about 2 percent by weight of the exogenous chemical, but for some purposes can contain up to about 10 percent by weight or even more of the exogenous chemical.

Alternatively, the composition can be a shelf-stable concentrate composition comprising the exogenous chemical substance in an amount of about 10 to about 90 percent by weight. By "shelf-stable" in this context it is meant that the composition does not exhibit phase separation when stored at ambient temperature for a period of time dependent on the particular circumstances. Such shelf-stable concentrates can be, for example, (1) a solid composition comprising the exogenous chemical substance in an amount of about 30 to about 90 percent by weight, such as a water-soluble or water-dispersible granular formulation, or (2) a composition that further comprises a liquid diluent, wherein the composition comprises the exogenous chemical substance in an amount of about 10 to about 60 percent by weight. In this latter embodiment, it is especially preferred for the exogenous chemical substance to be water-soluble and present in an aqueous phase of the composition in an amount of about 15 to about 45 percent by weight of the composition. In particular, such a composition can be, for example, an aqueous solution concentrate or an emulsion having an oil phase. If it is an emulsion, it can more specifically be, for example, an oil-in-water emulsion, a water-in-oil emulsion, or a water-in-oil-in-water multiple emulsion. In one particular embodiment of the invention, the solid or aqueous composition further comprises a solid inorganic particulate colloidal material.

As described above, one embodiment of the invention is a sprayable composition having the property that it forms anisotropic aggregates in or on a wax layer. This composition comprises an exogenous chemical, an aqueous diluent, and a first excipient substance which is amphiphilic. In the sprayable composition, the weight/weight ratio of the first excipient substance to the exogenous chemical is between about 1:3 and about 1:100. A sprayable composition conforms to this embodiment of the invention even if the formation of anisotropic aggregates in or on a wax layer occurs only following concentration of the composition on the wax layer by evaporation of water. The term "spray composition" is sometimes used herein to mean a sprayable composition.

In a related embodiment of the invention, a concentrate composition is provided which, upon dilution, dispersion or dissolution in water forms the sprayable composition just described. The concentrate composition contains a reduced amount of the aqueous diluent, or, in a particular embodiment, is a dry composition having less than about 5% water by weight. Typically a concentrate composition of the invention contains at least about 10% by weight of the exogenous chemical, preferably at least about 15%.

An alternative embodiment is a composition that does not itself comprise an exogenous chemical, but is intended for application to a plant in conjunction with or as a carrier for the application of an exogenous chemical. This composition comprises a first excipient substance as described above. Such a composition may be sprayable, in which case it also comprises an aqueous diluent, or it may be a concentrate, requiring dilution, dispersion or dissolution in water to provide a sprayable composition. Thus, this embodiment of the invention can be provided as a stand-alone product and applied to a plant, diluted as appropriate with water, simultaneously with the application of an exogenous chemical, or before or after the application of the exogenous chemical.

In all embodiments, it is believed that the first excipient substance forms supramolecular aggregates in aqueous solution or dispersion. In particular it is believed that aqueous compositions of the present invention form aggregates in aqueous solution or dispersion the majority of which are not simple micelles. "Majority" means that more than 50% by weight of the first excipient substance present is in the form of complex aggregates other than simple micelles, e.g. as bilayers or multilamellar structures. Preferably, more than 75% by weight is in the form of complex aggregates other than simple micelles.

Whether or not an amphiphilic substance forms such aggregates depends on its molecular architecture. The effects of molecular architecture on supramolecular self-assembly of amphiphilic molecules, as set forth for example by J. N. Israelachvili, D. J. Mitchell and B. W. Ninham in Faraday Transactions II, Volume 72, pp. 1525-1568 (1976) and in numerous later articles and monographs, are well known and understood. An important aspect is "critical packing parameter" (P) which is defined in the literature by the following equation:

    P=V/lA

where V is the volume of the hydrophobic tail of the molecule, l is the effective length of the hydrophobic tail, and A is the area occupied by the hydrophilic headgroup. These dimensions can be calculated from physical measurements as described in the literature and have been published for numerous amphiphilic compounds.

It is believed that amphiphilic substances useful as the first excipient substance herein have a critical packing parameter greater than 1/3. The first excipient substance forms aggregates in aqueous solution or dispersion which preferably have at least one dimension that is greater than two times the molecular length of the first excipient substance.

In one embodiment of the invention, an aqueous composition comprises supramolecular aggregates of the first excipient substance which have an average diameter of at least 20 nm, preferably at least 30 nm.

These supramolecular aggregates can take a number of forms. In one preferred embodiment, the first excipient substance is a vesicle-forming amphiphilic substance, such as a vesicle-forming lipid, and when the substance is dispersed in water the majority (greater than 50% by weight, preferably greater than 75% by weight) of the first excipient substance is present as vesicles or liposomes. In another preferred embodiment the first excipient substance is present as bilayers or multilamellar structures which are not organized as vesicles or liposomes. Compositions of the present invention can also include, without limitation, colloidal systems such as emulsions (water/oil, oil/water, or multiple, e.g., water/oil/water), foams, microemulsions, and suspensions or dispersions of microparticulates, nanoparticulates, or microcapsules. Compositions of the invention can include more than one type of aggregate or colloidal system; examples include liposomes or vesicles dispersed in a microemulsion, and compositions having characteristics of both emulsions and suspensions, e.g. suspo-emulsions. The present invention also encompasses any formulation, which may or may not contain a significant amount of water, that on dilution in an aqueous medium forms such colloidal systems, and/or systems comprising vesicles, liposomes, bilayers or multilamellar structures, so long as the other requirements stipulated herein are met.

The weight ratio of the first excipient substance to the exogenous chemical is between about 1:3 and about 11:100. We have been surprised by the high level of biological effectiveness, specifically herbicidal effectiveness of a glyphosate composition, exhibited at such low ratios of excipient substance to exogenous chemical. Higher ratios can also be effective but are likely to be uneconomic in most situations and increase the risk of producing an antagonistic effect on effectiveness of the exogenous chemical.

Prior art exogenous chemical compositions that have included liposome-forming excipient substances have typically contained a higher percentage of the liposome-forming excipient substance than of the exogenous chemical. Compositions of the present invention, in contrast, contain less of the excipient substance than the exogenous chemical, and in some embodiments much less. This makes the compositions of the present invention much less expensive than the above-described prior art compositions. It is surprising that the enhancement of biological activity that has been observed when using the present invention can be achieved with the addition of relatively small amounts of such excipient substances.

In one embodiment of the invention the first excipient substance is a liposome-forming material that comprises an amphiphilic compound or mixture of such compounds having two hydrophobic moieties, each of which is a saturated alkyl or acyl chain having from about 8 to about 22 carbon atoms. The amphiphilic compound or mixture of such compounds having said two hydrophobic moieties with about 8 to about 22 carbon atoms constitutes from about 40 to 100 percent by weight of all amphiphilic compounds having two hydrophobic moieties present in the liposome-forming material. Preferably the liposome-forming material has a hydrophilic head group comprising a cationic group. More preferably, the cationic group is an amine or ammonium group.

In a preferred embodiment of the invention, the first excipient substance comprises a liposome-forming compound having a hydrophobic moiety comprising two saturated or unsaturated hydrocarbyl groups R¹ and R² each having about 7 to about 21 carbon atoms. A number of subclasses of such liposome-forming compounds are known.

One subclass has the formula

    N.sup.+ (CH.sub.2 R.sup.1)(CH.sub.2 R.sup.2)(R.sup.3)(R.sup.4)Z.sup.-I

wherein R³ and R⁴ are independently hydrogen, C₁₋₄ alkyl or C₁₋₄ hydroxyalkyl and Z is a suitable anion.

A second subclass has the formula

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH(OCH.sub.2 R.sup.1)CH.sub.2 (OCH.sub.2 R.sup.2)Z.sup.-                                II

wherein R⁵, R⁶ and R⁷ are independently hydrogen, C₁₋₄ alkyl or C₁₋₄ hydroxyalkyl and Z is a suitable anion.

A third subclass has the formula

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH(OCOR.sup.1)CH.sub.2 (OCOR.sup.2)Z.sup.-                                       III

wherein R⁵, R⁶, R⁷ and Z are as defined above.

A fourth subclass has the formula

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH.sub.2 --PO.sub.4.sup.- --CH.sub.2 CH(OCOR.sup.1)CH.sub.2 (OCOR.sup.2)            IV

wherein R⁵, R⁶, and R⁷ are as defined above.

Compounds of formulas I-IV will have the indicated formulas at a pH of 4 and may have the same formulas at other pH's as well. It should be understood, however, that compositions of the present invention are not limited to use at a pH of 4.

R¹ and R² preferably are independently saturated straight-chain alkyl groups each having about 7 to about 21 carbon atoms. Examples of suitable agriculturally acceptable anions Z include hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.

In all of the above subclasses of liposome-forming substances, the hydrophilic moiety comprises a cationic group, specifically an amine or ammonium group. The compound as a whole is in some cases cationic (as in I, II and III) and in some cases neutral (as in IV). Where the amine group is quaternary, it behaves as a cationic group independently of pH. Where the amine group is secondary or tertiary, it behaves as a cationic group when protonated, i.e. in an acid medium, for example at a pH of 4.

In a preferred embodiment, the first excipient substance is a phospholipid selected from the group consisting of di-C₈₋₂₂ -alkanoylphosphatidylcholines and di-C₈₋₂₂ -alkanoylphosphatidylethanolamines. In a particularly preferred embodiment, the first excipient substance is a dipalmitoyl or distearoyl ester of phosphatidylcholine or a mixture thereof.

Other subclasses of liposome-forming substances having two hydrophobic chains each comprising a C₇₋₂₁ hydrocarbyl group can also be used as the first excipient substance in compositions of the invention. While substances having a cationic group in the hydrophilic moiety are preferred, nonionic or anionic substances can be used if desired.

In another embodiment of the invention, the first excipient substance is an amphiphilic quaternary ammonium compound or mixture of such compounds. The hydrophobic moiety of the quaternary ammonium compound is a saturated alkyl or haloalkyl group having about 6 to about 22 carbon atoms. In this embodiment, the first excipient substance is not necessarily a liposome-forming substance, but it is believed to form aggregates in aqueous solution or dispersion as described above.

Preferred quaternary ammonium compounds (other than those which are liposome-forming and have two hydrocarbyl chains) for use as the first excipient substance in compositions of the invention have the formula

    R.sup.8--W.sub.a --X--Y.sub.b --(CH.sub.2).sub.n --N.sup.+ (R.sup.9)(R.sup.10)(R.sup.11)T.sup.-                      V

wherein R⁸ represents the hydrophobic moiety and is a hydrocarbyl or haloalkyl group having from about 6 to about 22 carbon atoms, W and Y are independently O or NH, a and b are independently 0 or 1 but at least one of a and b is 1, X is CO, SO or SO₂, n is 2 to 4, R⁹, R¹⁰ and R¹¹ are independently C₁₋₄ alkyl, and T is a suitable anion. R⁸ in one particular embodiment is hydrocarbyl having about 12 to about 18 carbon atoms. R⁸ can also be fluorinated. In one specific embodiment, R⁸ is perfluorinated, and preferably has about 6 to about 12 carbon atoms. Suitable anions T include hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate. In one particularly preferred embodiment, R⁸ is saturated perfluoroalkyl having about 6 to about 12 carbon atoms, X is CO or SO₂, Y is NH, a is 0, b is 1, n is 3, R⁹, R¹⁰ and R¹¹ are methyl, and T is selected from the group consisting of chloride, bromide and iodide.

In a further embodiment of the invention, the first excipient substance is an alkylether surfactant or mixture of such surfactants having the formula

    R.sup.12 --O--(CH.sub.2 CH.sub.2 O).sub.n (CH(CH.sub.3)CH.sub.2 O).sub.m --R.sup.13                                                VI

wherein R¹² is an alkyl or alkenyl group having about 16 to about 22 carbon atoms, n is an average number of about 10 to about 100, m is an average number of 0 to about 5 and R¹³ is hydrogen or C₁₋₄ alkyl. Preferably R¹² is a saturated straight-chain alkyl group, R¹³ is hydrogen, m is 0 and n is from about 10 to about 40, more preferably from about 20 to about 40. Most preferably the alkylether surfactant is a polyoxyethylene cetyl or stearyl ether or mixture thereof having 20-40 moles of ethylene oxide (EO). The term "alkylether" as used herein should be understood to include alkenylether surfactants.

Compositions of the present invention can optionally further comprise a second excipient substance having at least one hydrophobic moiety, wherein if the second excipient substance has one hydrophobic moiety, the hydrophobic moiety is a hydrocarbyl or haloalkyl group having about 6 to about 22 carbon atoms, and wherein if the second excipient substance has a plurality of hydrophobic moieties, each such hydrophobic moiety is a hydrocarbyl or haloalkyl group having more than 2 carbon atoms, said plurality of hydrophobic moieties having a total of about 12 to about 40 carbon atoms. The second excipient substance, if present, may or may not itself be one that forms supramolecular aggregates as described above. In a particular embodiment of the invention where the first excipient substance is a liposome-forming substance of formula I, II, III or IV above, a second excipient substance is present and is a quaternary ammonium compound or mixture of such compounds. Among preferred quaternary ammonium compounds for use as the second excipient substance in this embodiment are compounds of formula V above.

In another particular embodiment of the invention where the first excipient substance is a liposome-forming substance of formula I, II, III or IV above, a second excipient substance is present and is a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15                                 VII

wherein R¹⁴ is a hydrocarbyl group having about 5 to about 21 carbon atoms, R¹⁵ is a hydrocarbyl group having 1 to about 14 carbon atoms, the total number of carbon atoms in R¹⁴ and R¹⁵ is about 11 to about 27, and A is O or NH.

R¹⁴ preferably has about 11 to about 21 carbon atoms, R¹⁵ preferably has 1 to about 6 carbon atoms and A is preferably O. More preferably, the second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ fatty acid, for example a propyl, isopropyl or butyl ester of a C₁₂₋₁₈ fatty acid. Butyl stearate is an especially preferred example. The aqueous composition in embodiments comprising a compound of formula VII preferably is an emulsion comprising an oil phase that comprises said second excipient substance, for example a water-in-oil-in-water multiple emulsion or an oil-in-water emulsion. Alternatively, a second excipient substance of formula VII is associated in some way with a liposome-forming first excipient substance.

In yet another particular embodiment of the invention, the first excipient substance is an alkylether surfactant of formula VI and a second excipient substance is present and is a compound or mixture of compounds of formula VII.

In any of the above particular embodiments, the exogenous chemical and/or second excipient substance can be encapsulated within or associated with aggregates (e.g., liposomes) formed by the first excipient substance, but do not necessarily have to be so encapsulated or associated. "Associated" in this context means bound to or at least partly intercalated in some fashion in a vesicle wall, as opposed to being encapsulated. In yet another embodiment of the invention where the first excipient substance forms liposomes, the exogenous chemical and/or second excipient substance is not encapsulated in or associated with the liposomes at all. Although the present invention does not exclude the possibility of so encapsulating or associating the exogenous chemical, a presently preferred dilute sprayable liposomal composition encapsulates less than 5% by weight of the exogenous chemical that is present in the overall composition. Another dilute sprayable liposomal embodiment of the present invention has no substantial amount (i.e., less than 1% by weight) of the exogenous chemical encapsulated in the liposomes. As a droplet of such a liposomal composition dries on foliage of a plant, the proportion of the exogenous chemical that is encapsulated in the liposomes may change. Compositions of the present invention that include an exogenous chemical can be applied to foliage of plants in an amount that is effective to achieve the desired biological effect of the exogenous chemical. For example, when the exogenous chemical is a post-emergence herbicide, the composition can be applied to a plant in a herbicidally effective amount.

Without being bound by theory, it is believed that that the method and compositions of the present invention create or enlarge hydrophilic channels through the epicuticular wax of the plant cuticle, these channels being capable of accommodating the mass transfer of a water-soluble exogenous chemical into the plant, and thus transporting the exogenous chemical into the plant more rapidly or more completely than an epicuticular wax layer lacking such formation or enlargement of hydrophilic channels. Of course, certain compositions of the present invention can also enter a plant through stomata, but this generally requires a very low surface tension which is not an essential feature of the present compositions. The enhanced cuticular penetration believed to be achieved by the compositions of the present invention enhances the overall delivery and effectiveness of the exogenous chemical. Whereas an exogenous chemical such as glyphosate, formulated as an aqueous solution or dispersion with surfactants which do not have the property of forming anisotropic aggregates in or on a wax layer, normally penetrates through the epicuticular wax very slowly (e.g., in 1-4 days), a substantial portion of the exogenous chemical in compositions of the present invention penetrates much more quickly (e.g., in from about 10 minutes to a few hours, preferably in less than about 30 minutes).

Thus, methods and compositions of the invention are believed to owe their superior effectiveness at least in part to accelerated uptake into plant foliage. In conventional methods of treating plants with exogenous chemicals, in particular polar exogenous chemicals, the epicuticular wax layer presents an almost continuous barrier through which such exogenous chemicals diffuse with difficulty, even in the presence of surfactants which increase diffusive mobility but do not introduce the possibility of rapid mass transfer through hydrophilic channels.

Again without being bound by theory, it is believed that the hydrophilic channels are created within the epicuticular wax layer by the self-assembly of molecules of the first excipient substance which has a hydrophobic moiety that associates with the wax and a hydrophilic moiety that attracts water to form an aqueous continuum across the epicuticular wax layer linking up with hydrophilic pathways in the cuticle proper. A polar exogenous chemical can move by mass transfer along such an aqueous continuum to enter the plant.

Again without being bound by theory, it is believed that when the composition is present on the leaf of a plant as a droplet of aqueous solution or dispersion, in an aqueous microdomain on the cuticular surface (i.e., the aqueous region at the interface between the water droplet and the epicuticular wax), the majority (i.e., more than 50% by weight) of the aggregate-forming substance is present in a form other than a monolayer, for example as a bilayer or multilamellar (liquid crystal) structure. The aggregate-forming substances employed have several preferred characteristics that are believed to contribute to the formation of transcuticular hydrophilic channels. For instance, they have a tendency to form extended self-assembled structures in the presence of water and the kinds of waxes encountered in cuticles. Generally, materials that form non-simple (i.e., not small spherical micellar structures) aggregates in solution, such as vesicles or cylindrical, discotic, or ribbon-like micellar structures are preferred. These tend to form more complex adsorbed and absorbed layers with hydrophobic substrates than those simple micellar systems that tend to produce simple adsorbed monolayers. These substances also tend to produce lyotropic mesophases such as lamellar, hexagonal or reversed hexagonal phases in the compositions established in the aqueous microdomains in or on the cuticle.

In one embodiment of the invention, a cationic headgroup on the first excipient substance is also preferred. The cationic group is believed to enhance initial adhesion to the leaf surface, since the majority of such surfaces carry an overall negative charge. The cationic group is also believed to contribute to the hydrophilicity of channels in the epicuticular wax formed or enlarged by the method and compositions of the invention. Cationic groups, in particular amine or ammonium groups, attract water molecules which further enlarge the hydrophilic channels and thereby provide an improved pathway of entry for exogenous chemicals that are polar or water-soluble.

It is further believed that the creation or enlargement of hydrophilic channels in epicuticular wax results in the wax becoming plasticized. A further embodiment of the invention is thus a method for applying an exogenous chemical to a plant having an epicuticular wax layer, comprising (a) plasticizing the epicuticular wax layer in conjunction with (b) contacting the epicuticular wax layer with the exogenous chemical. In this embodiment the step of plasticizing the epicuticular wax layer is accomplished by contacting the layer with an aqueous composition comprising a first excipient substance as defined above and optionally a second excipient substance as defined above. The weight ratio of the first excipient substance to the exogenous chemical is between about 1:3 and about 1:100.

Herbicidal compositions in accordance with the present invention are also useful in methods for enhancing the yield of a field crop. Such a method can comprise the steps of (a) planting a crop in a field, (b) substantially freeing the field of one or more weed species that would diminish the yield of the crop by applying to the weed species a herbicidally effective amount of a composition as described above, (c) allowing the crop to mature, and (d) harvesting the crop. Alternatively, the method can comprise the steps of (a) substantially freeing the field of one or more weed species that would diminish the yield of the crop by applying to the weed species a herbicidally effective amount of the composition, (b) planting the crop in the field, (c) allowing the crop to mature, and (d) harvesting the crop.

In one particular method in accordance with the present invention, a herbicidal composition as described above can be applied to a complex of weeds that are present in a single field, the weeds being, for example, velvetleaf, morningglory, and prickly sida. The composition is applied in a herbicidally effective amount, and provides herbicidal control of each of the weed species in the complex.

Another embodiment of the present invention is a herbicidal method, comprising contacting the foliage of a plant with a herbicidally effective amount of a composition as described above, whereby the herbicidal effectiveness of the composition on the plant to which it is applied is visibly better than the herbicidal effectiveness on that same species of plant, under substantially the same conditions, of a composition containing a similar amount of surfactant but that does not form anisotropic aggregates. "Visibly better" in this context means that the difference in herbicidal effect of the two compositions on the plants is readily noticeable to the eye of an experienced weed scientist.

Another embodiment of the present invention is a herbicidal method which can be used in a field that contains both weed and crop plants, where the crop plants are resistant to the effects of a particular herbicide at the rate that herbicide is used. The method comprises contacting the foliage of both the weeds and the crops in the field with a composition as described above. The composition will have a herbicidal effect on the weeds (i.e., it will partially or entirely kill the weeds) but it will not harm the crops. This herbicidal method applies to any combination of a selective post-emergence herbicide (e.g. 2,4-D) and a crop on which that herbicide can be used selectively to kill weeds (e.g., in the case of 2,4-D, wheat). This herbicidal method also applies to any combination of a normally non-selective post-emergence herbicide and a crop bred or genetically modified to be resistant to that herbicide. An example of a suitable combination of herbicide and herbicide-resistant crop is ROUNDUP® herbicide and ROUNDUP READY® crops, developed by Monsanto Company.

The compositions and methods of the present invention have a number of advantages. They provide enhanced biological activity of exogenous chemicals in or on plants in comparison with prior formulations, either in terms of greater ultimate biological effect, or obtaining an equivalent biological effect while using a reduced application rate of exogenous chemical. Certain herbicide formulations of the present invention can avoid antagonism that has been observed in some prior art herbicide formulations, and can minimize quick production of necrotic lesions on leaves that in some situations hinder overall translocation of herbicide in the plant. Certain herbicide compositions of the invention modify the spectrum of activity of the herbicide across a range of plant species. For example, certain formulations of the present invention containing glyphosate can provide good herbicidal activity against broadleaf weeds while not losing any herbicidal effectiveness on narrowleaf weeds. Others can enhance herbicidal effectiveness on narrowleaf weeds to a greater extent than on broadleaf weeds. Still others can have enhanced effectiveness which is specific to a narrow range of species or even a single species.

Another advantage of the present invention is that it employs relatively small amounts of the first and second excipient substances in relation to the amount of exogenous chemical employed. This makes the compositions and methods of the present invention relatively inexpensive, and also tends to reduce instability problems in specific compositions where one or both excipient substances are physically incompatible with the exogenous chemical (e.g., alkylether surfactants in solutions of high ionic strength, such as concentrated glyphosate salt solutions).

Even at the low concentrations of the excipient substances used in the present invention, there may be limits on the maximum concentration of exogenous chemical that can be used without causing compatibility problems (e.g., separation of the composition into discrete layers). In some preferred embodiments of the invention, composition stability at high loadings of exogenous chemical is maintained by adding other ingredients such as, for example, colloidal particulates. Some compositions of the present invention exhibit enhanced biological activity and have a higher loading of exogenous chemical than possible in prior art compositions.

Further, compositions of the present invention are less sensitive in some instances to environmental conditions such as relative humidity at the time of application to the plant. Also, the present invention allows the use of smaller amounts of herbicides or other pesticides, while still obtaining the required degree of control of weeds or other undesired organisms.

DESCRIPTION OF SPECIFIC EMBODIMENTS

When the phrase "anisotropic aggregates in or on a wax layer" is used herein, it relates to determinations made by the following test procedure. We have found this test to predict with a high degree of reliability whether a composition comprising water and an exogenous chemical, or a composition comprising water which is to be used in conjunction with an exogenous chemical, will show enhanced biological effectiveness when applied to foliage of plants. Modifications can be made to the test; however a procedure modified in some major respect will not necessarily give the same results and will not necessarily predict enhanced effectiveness as reliably as the procedure described here.

The first stage in the procedure is to prepare a wax-coated slide. We have found a preferred wax for the purpose to be a blend of carnauba wax and beeswax in a weight/weight ratio of approximately 10:1. A clear wax mixture is prepared consisting of 5% carnauba wax and 0.5% beeswax in isopropanol, and is maintained at a temperature of approximately 82° C. The end of a glass 2.4 cm×7.2 cm microscope slide is immersed perpendicularly in the wax mixture to a depth of approximately one-third of the length of the slide. After 10 to 15 seconds, the slide is very slowly and steadily withdrawn from the wax mixture and allowed to cool, leaving a wax layer deposited on both faces of the slide.

Visual examination of the slide can give a preliminary indication of the thickness and uniformity of the wax coating. If imperfections are evident the slide is rejected. If the slide shows no obvious imperfections, the wax coating is carefully removed from one face of the slide by wiping with acetone. Further evaluation of the acceptability of the wax-coated slide for the test is done by examining the slide under a microscope. The slide is selected for use in the test if, on microscopic examination using a 4.9× objective, the wax coating is uniformly thick and there is uniform density of wax particles across the slide. Preference is for a coating that has few observable wax particles and exhibits a very dark field when examined under polarized light.

The next stage in the procedure is to conduct the test. For this purpose, samples of an exogenous chemical composition to be tested are diluted, if necessary, to 15% to 20% by weight of the exogenous chemical. In the case of glyphosate, the desired concentration in a composition sample is 15% to 20% acid equivalent (a.e.). Samples of reference compositions are also prepared; in the case of glyphosate, Formulations B and J as defined in the Examples herein are appropriate.

For a composition of a first excipient substance not containing an exogenous chemical but to be applied in conjunction with an exogenous chemical, the desired concentration is approximately 5% to 7% by weight of the first excipient substance.

The following instrumentation, or equivalent, items are required or useful:

Nikon SMZ-10A stereoscopic microscope equipped for polarized light observation, photomicrography, and video observation and recording.

3CCD MTI camera.

Diagnostic Instruments 150 IL-PS power supply.

Sony Trinitron color video monitor, model PVM-1353MD.

Mitsubishi time-lapse video cassette recorder, model HS-S5600.

Hewlett Packard Pavillion 7270 computer, with Windows 95 and Image-Pro Plus version 2.0 electronic imaging program installed.

Hewlett Packard Deskjet 870Cse printer.

A wax-coated slide, prepared and selected as described above, is positioned on the microscope stage, with the system set to provide transmitted light, both straight and polarized. A 1 μl drop of the sample to be tested is applied to the wax surface using a thoroughly cleaned 1 μl Hamilton syringe. This and subsequent operations are followed through the microscope at 4.9× objective. Duplicate or triplicate tests are done for each composition. Numerous tests can be conducted simultaneously on a single slide. Progression of change in the microscopic appearance of the sample is observed through the microscope and recorded at designated time intervals. We have found useful intervals to be 1 minute, 10 minutes, 2 hours and >24 hours after application of the drop to the wax surface. Observations can also be made at intermediate times to capture possible significant transitions occurring at such times.

The temperature of the wax layer tends to increase with prolonged exposure to the microscope light. In many cases we have found this does not significantly interfere with the results obtained. However, in some cases temperature does affect the outcome of the test and in such cases it is preferred to illuminate the sample only for the short periods necessary to make observations, so that the temperature of the wax layer remains close to ambient temperature. An example of a composition of the invention where it is believed to be important to keep temperature close to ambient is one containing a fatty acid ester such as butyl stearate.

At dark field (polarized light) the wax layer is observed for birefringence, and at light field the character of the drop surface is observed, at each time interval. The following records are made:

birefringence (yes/no);

time of initial appearance of birefringence;

character of the birefringence;

appearance of drop surface as composition "dries";

degree of spread of the drop;

effects of temperature (warming of the slide) if any;

other noticeable changes.

Optionally, images are recorded at significant times using the 3CCD MTI camera and the Image-Pro Plus program as documentation of observed changes. Tests may if desired also be recorded on video, especially during the first 15 minutes. In addition to images captured using 4.9× objective, overall-field views using 0.75× objective can be recorded to provide clear comparisons of different samples tested on the same slide.

A particularly useful parameter for predicting enhanced effectiveness is the observation of birefringence (yes/no) 5-20 minutes after deposition of the test drop on the wax-coated slide. We have found 10-15 minutes after deposition to be an especially suitable time for observation of this parameter. The following results for oil-in-water emulsion compositions comprising glyphosate IPA salt, butyl stearate and alkylether surfactants are typical of those obtained. Each of compositions WCS-1 to WCS-5 contained 15% w/w glyphosate a.e., 0.5% w/w butyl stearate and 5% w/w alkylether surfactant. Formulations B and J are commercial standard compositions of glyphosate defined in the Examples section later herein, and were diluted to 15% glyphosate a.e. for the test.

    ______________________________________                                                                      Birefringence                                       Composition Alkylether at 10 min                                             ______________________________________                                         WCS-1    Brij 78 (steareth-20)                                                                              yes                                                 WCS-2 Plurafac A-38 (ceteareth-27) yes                                         WCS-3 Brij 98 (oleth-20) yes                                                   WCS-4 Brij 35 (laureth-23) no                                                  WCS-5 Neodol 1-9 (C.sub.11 linear alcohol 9E0) no                              Formulation B  no                                                              Formulation J  no                                                            ______________________________________                                    

It will be noted that where the hydrophobic moiety of the alkylether was a C₁₁ (WCS-5) or C₁₂ (WCS-4) hydrocarbyl group, the composition did not show anisotropic properties in the form of birefringence 10 minutes after application to the wax-coated slide. However, where the hydrophobic moiety had a carbon chain length of 16 to 18 (WCS-1 to WCS-3), birefringence was evident, indicating the presence of anisotropic aggregates in or on the wax layer. The intensity of birefringence was greatest with WCS-1 (containing steareth-20), followed by WCS-2 (containing ceteareth-27) and then WCS-3 (oleth-20).

Tests of alkylether compositions, as evidenced in Examples herein, have shown that in general those containing alkylethers of hydrophobe carbon chain length 16 or greater show greater biological effectiveness than those having a shorter hydrophobe. In general greater biological effectiveness has been obtained where the hydrophobe is saturated (as, for example, in steareth-20 and ceteareth-27) than where it is unsaturated (as, for example, in oleth-20).

The following compositions were made containing 15% glyphosate a.e. and 5% alkylether surfactant, but no butyl stearate. In WCS-10 the surfactant was steareth-10, in WCS-11 oleth-10 and in WCS-12 steareth-8 (laboratory sample from Sigma).

    ______________________________________                                                                   Birefringence                                          Composition Alkylether at 15 min                                             ______________________________________                                         WCS-10       Brij 76 (steareth-10)                                                                       yes                                                    WCS-11 Brij 97 (oleth-10) no                                                   WCS-12 steareth-8 yes                                                        ______________________________________                                    

The property of forming anisotropic aggregates as determined by this test appears to require, on a C₁₆₋₁₈ straight-chain alcohol, a minimum of about 10 moles of ethylene oxide (EO). Where the alcohol is oleyl, an EO chain of 10 units is already too short, but where the alcohol is stearyl, even as short an EO chain as 8 units appears to suffice. It should be noted, however, that the steareth-8 used in composition WCS-12 was obtained as a laboratory sample and is likely chemically purer than the commercial surfactants used in other compositions. Commercial grade steareth-8 will not necessarily give the same result.

As further evidence of the usefulness of the present anisotropy test in predicting biological effectiveness of exogenous chemical compositions, compositions WCS-6, WCS-7 and WCS-8 were prepared, each containing 30% glyphosate a.e. by weight, and were then diluted to 15% glyphosate a.e. for the test. All contained soybean lecithin (45% phospholipid, Avanti) and were prepared by process (v) as detailed in the Examples herein. Composition WCS-6, before dilution, contained 5% lecithin, 5% Fluorad FC-754 and 0.75% Ethomeen T/25. Composition WCS-7, before dilution, contained 2% lecithin and 2% Fluorad FC-754. Composition WCS-8, before dilution, contained 2% lecithin and 0.75% Ethomeen T/25. In addition, Composition WCS-9 was prepared containing 15% glyphosate a.e. and 5% soybean lecithin (45% phospholipid, Avanti). The following results were obtained.

    ______________________________________                                                                      Birefringence                                       Composition Excipient ingredients at 10 min.                                 ______________________________________                                         WCS-6    lecithin + FC-754 + Ethomeen T125                                                                  yes                                                 WCS-7 lecithin + FC-754 yes                                                    WCS-8 lecithin + Ethomeen T/25 no                                              WCS-9 lecithin no                                                            ______________________________________                                    

As evidenced in the Examples herein, enhanced biological effectiveness is a feature of compositions containing lecithin as the first excipient substance and Fluorad FC-754 as the second excipient substance. In the absence of Fluorad FC-754 or like material, lecithin, either alone or together with a tertiary alkylamine surfactant such as Ethomeen T/25 or MON 0818, does not consistently generate the desired enhancement.

In a further demonstration of the usefulness of the present anisotropy test, compositions WCS-13 and WCS-14 were prepared, each containing 20% glyphosate a.e. by weight, and were then diluted to 15% glyphosate a.e. for the test. Both contained soybean lecithin (45% phospholipid, Avanti). Composition WCS-13 was made by process (x) as described in the Examples herein and, before dilution, contained 6% lecithin, 6% Ethomeen T/25 and 1.5% butyl stearate. Composition WCS-14 was identical except that it contained no butyl stearate. Particular care was taken in this study to avoid excessive warming of the wax-coated slide by prolonged illumination. The following results were obtained.

    ______________________________________                                                                       Birefringence                                      Composition Excipient ingredients at 15 min.                                 ______________________________________                                         WCS-13  lecithin + Ethomeen T/25 + butyl stearate                                                            yes                                                WCS-14 lecithin + Ethomeen T/25 no                                           ______________________________________                                    

The addition of a small quantity of butyl stearate was thus sufficient to confer, on a glyphosate+lecithin+Ethomeen T/25 composition, the property of forming anisotropic aggregates in or on a wax layer. The Examples herein illustrate the unexpected enhancement of biological effectiveness observed when an exogenous chemical is formulated with lecithin and a fatty acid ester such as butyl stearate.

Thus where, for reasons of economy, compatibility with the exogenous chemical, or other considerations it is desired to provide an exogenous chemical composition having a relatively low content of excipient substances (for example a weight ratio of each excipient substance to exogenous chemical of about 1:3 or less), the anisotropy test provided here is an in vitro assay method which can be used to identify biologically effective compositions in advance of extensive testing in vivo.

The in vitro assay method just described, together with modifications thereof that will be readily apparent to those of skill in the art, is a further embodiment of the present invention.

Examples of exogenous chemical substances that can be included in compositions of the present invention include, but are not limited to, chemical pesticides (such as herbicides, algicides, fungicides, bactericides, viricides, insecticides, aphicides, miticides, nematicides, molluscicides and the like), plant growth regulators, fertilizers and nutrients, gametocides, defoliants, desiccants, mixtures thereof and the like. In one embodiment of the invention, the exogenous chemical is polar.

A preferred group of exogenous chemicals are those that are normally applied post-emergence to the foliage of plants, i.e. foliar-applied exogenous chemicals.

Some exogenous chemicals useful in the present invention are water-soluble, for example salts that comprise biologically active ions, and also comprise counterions, which may be biologically inert or relatively inactive. A particularly preferred group of these water-soluble exogenous chemicals or their biologically active ions or moieties are systemic in plants, that is, they are to some extent translocated from the point of entry in the foliage to other parts of the plant where they can exert their desired biological effect. Especially preferred among these are herbicides, plant growth regulators and nematicides, particularly those that have a molecular weight, excluding counterions, of less than about 300. More especially preferred among these are exogenous chemical compounds having one or more functional groups selected from amine, carboxylate, phosphonate and phosphinate groups.

Among such compounds, an even more preferred group are herbicidal or plant growth regulating exogenous chemical compounds having at least one of each of amine, carboxylate, and either phosphonate or phosphinate functional groups. Salts of N-phosphonomethylglycine are examples of this group of exogenous chemicals. Further examples include salts of glufosinate, for instance the ammonium salt (ammonium DL-homoalanin-4-yl (methyl) phosphinate).

Another preferred group of exogenous chemicals which can be applied by the method of the invention are nematicides such as those disclosed in U.S. Pat. No. 5,389,680, the disclosure of which is incorporated herein by reference. Preferred nematicides of this group are salts of 3,4,4-trifluoro-3-butenoic acid or of N-(3,4,4-trifluoro-1-oxo-3-butenyl)glycine.

Exogenous chemicals which can usefully be applied by the method of the present invention are normally, but not exclusively, those which are expected to have a beneficial effect on the overall growth or yield of desired plants such as crops, or a deleterious or lethal effect on the growth of undesirable plants such as weeds. The method of the present invention is particularly useful for herbicides, especially those that are normally applied post-emergence to the foliage of unwanted vegetation.

Herbicides which can be applied by the method of the present invention include but are not limited to any listed in standard reference works such as the "Herbicide Handbook," Weed Science Society of America, 1994, 7th Edition, or the "Farm Chemicals Handbook," Meister Publishing Company, 1997 Edition. Illustratively these herbicides include acetanilides such as acetochlor, alachlor and metolachlor, aminotriazole, asulam, bentazon, bialaphos, bipyridyls such as paraquat, bromacil, cyclohexenones such as clethodim and sethoxydim, dicamba, diflufenican, dinitroanilines such as pendimethalin, diphenylethers such as acifluorfen, fomesafen and oxyfluorfen, fatty acids such as C₉₋₁₀ fatty acids, fosamine, flupoxam, glufosinate, glyphosate, hydroxybenzonitriles such as bromoxynil, imidazolinones such as imazaquin and imazethapyr, isoxaben, norflurazon, phenoxies such as 2,4-D, phenoxypropionates such as diclofop, fluazifop and quizalofop, picloram, propanil, substituted ureas such as fluometuron and isoproturon, sulfonylurcas such as chlorimuron, chlorsulfuron, halosulfuron, metsulfuron, primisulfuron, sulfometuron and sulfosulfuron, thiocarbamates such as triallate, triazines such as atrazine and metribuzin, and triclopyr. Herbicidally active derivatives of any known herbicide are also within the scope of the present invention. A herbicidally active derivative is any compound which is a minor structural modification, most commonly but not restrictively a salt or ester, of a known herbicide. These compounds retain the essential activity of the parent herbicide, but may not necessarily have a potency equal to that of the parent herbicide. These compounds may convert to the parent herbicide before or after they enter the treated plant. Mixtures or coformulations of a herbicide with other ingredients, or of more than one herbicide, may likewise be employed.

An especially preferred herbicide is N-phosphonomethylglycine (glyphosate), a salt, adduct or ester thereof, or a compound which is converted to glyphosate in plant tissues or which otherwise provides glyphosate ion. Glyphosate salts that can be used according to this invention include but are not restricted to alkali metal, for example sodium and potassium, salts; ammonium salt; alkylamine, for example dimethylamine and isopropylamine, salts; alkanolamine, for example ethanolamine, salts; alkylsulfonium, for example trimethylsulfonium, salts; sulfoxonium salts; and mixtures thereof. The herbicidal compositions sold by Monsanto Company as ROUNDUP® and ACCORD® contain the monoisopropylamine (IPA) salt of N-phosphonomethylglycine. The herbicidal compositions sold by Monsanto Company as ROUNDUP® Dry and RIVAL® contain the monoammonium salt of N-phosphonomethylglycine. The herbicidal composition sold by Monsanto Company as ROUNDUP® Geoforce contains the monosodium salt of N-phosphonomethylglycine. The herbicidal composition sold by Zeneca as TOUCHDOWN® contains the trimethylsulfonium salt of N-phosphonomethylglycine. The herbicidal properties of N-phosphonomethylglycine and its derivatives were first discovered by Franz, then disclosed and patented in U.S. Pat. No. 3,799,758, issued Mar. 26, 1974. A number of herbicidal salts of N-phosphonomethylglycine were patented by Franz in U.S. Pat. No. 4,405,531, issued Sep. 20, 1983. The disclosures of both of these patents are hereby incorporated by reference.

Because the commercially most important herbicidal derivatives of N-phosphonomethylglycine are certain salts thereof, the glyphosate compositions useful in the present invention will be described in more detail with respect to such salts. These salts are well known and include ammonium, IPA, alkali metal (such as the mono-, di-, and trisodium salts, and the mono-, di-, and tripotassium salts), and trimethylsulfonium salts. Salts of N-phosphonomethylglycine are commercially significant in part because they are water soluble. The salts listed immediately above are highly water soluble, thereby allowing for highly concentrated solutions that can be diluted at the site of use. In accordance with the method of this invention as it pertains to glyphosate herbicide, an aqueous solution containing a herbicidally effective amount of glyphosate and other components in accordance with the invention is applied to foliage of plants. Such an aqueous solution can be obtained by dilution of a concentrated glyphosate salt solution with water, or dissolution or dispersion in water of a dry (e.g. granular, powder, tablet or briquette) glyphosate formulation.

Exogenous chemicals should be applied to plants at a rate sufficient to give the desired biological effect. These application rates are usually expressed as amount of exogenous chemical per unit area treated, e.g. grams per hectare (g/ha). What constitutes a "desired effect" varies according to the standards and practice of those who investigate, develop, market and use a specific class of exogenous chemicals. For example, in the case of a herbicide, the amount applied per unit area to give 85% control of a plant species as measured by growth reduction or mortality is often used to define a commercially effective rate.

Herbicidal effectiveness is one of the biological effects that can be enhanced through this invention. "Herbicidal effectiveness," as used herein, refers to any observable measure of control of plant growth, which can include one or more of the actions of (1) killing, (2) inhibiting growth, reproduction or proliferation, and (3) removing, destroying, or otherwise diminishing the occurrence and activity of plants.

The herbicidal effectiveness data set forth herein report "inhibition" as a percentage following a standard procedure in the art which reflects a visual assessment of plant mortality and growth reduction by comparison with untreated plants, made by technicians specially trained to make and record such observations. In all cases, a single technician makes all assessments of percent inhibition within any one experiment or trial. Such measurements are relied upon and regularly reported by Monsanto Company in the course of its herbicide business.

The selection of application rates that are biologically effective for a specific exogenous chemical is within the skill of the ordinary agricultural scientist. Those of skill in the art will likewise recognize that individual plant conditions, weather and growing conditions, as well as the specific exogenous chemical and formulation thereof selected, will affect the efficacy achieved in practicing this invention. Useful application rates for exogenous chemicals employed can depend upon all of the above conditions. With respect to the use of the method of this invention for glyphosate herbicide, much information is known about appropriate application rates. Over two decades of glyphosate use and published studies relating to such use have provided abundant information from which a weed control practitioner can select glyphosate application rates that are herbicidally effective on particular species at particular growth stages in particular environmental conditions.

Herbicidal compositions of glyphosate or derivatives thereof are used to control a very wide variety of plants worldwide. Such compositions can be applied to a plant in a herbicidally effective amount, and can effectively control one or more plant species of one or more of the following genera without restriction: Abutilon, Amaranthus, Artemisia, Asclepias, Avena, Axonopus, Borreria, Brachiaria, Brassica, Bromus, Chenopodium, Cirsium, Commelina, Convolvulus, Cynodon, Cyperus, Digitaria, Echinochloa, Eleusine, Elymus, Equisetum, Erodium, Helianthus, Imperata, Ipomoea, Kochia, Lolium, Malva, Oryza, Ottochloa, Panicum, Paspalum, Phalaris, Phragmites, Polygonum, Portulaca, Pteridium, Pueraria, Rubus, Salsola, Setaria, Sida, Sinapis, Sorghum, Triticum, Typha, Ulex, Xanthium, and Zea.

Particularly important species for which glyphosate compositions are used are exemplified without limitation by the following:

Annual broadleaves:

velvetleaf (Abutilon theophrasti)

pigweed (Amaranthus spp.)

buttonweed (Borreria spp.)

oilseed rape, canola, indian mustard, etc. (Brassica spp.)

commelina (Commelina spp.)

filaree (Erodium spp.)

sunflower (Helianthus spp.)

morningglory (Ipomoea spp.)

kochia (Kochia scoparia)

mallow (Malva spp.)

wild buckwheat, smartweed, etc. (Polygonum spp.)

purslane (Portulaca spp.)

russian thistle (Salsola spp.)

sida (Sida spp.)

wild mustard (Sinapis arvensis)

cocklebur (Xanthium spp.)

Annual narrowleaves:

wild oat (Avena fatua)

carpetgrass (Axonopus spp.)

downy brome (Bromus tectorum)

crabgrass (Digitaria spp.)

barnyardgrass (Echinochloa crus-galli)

goosegrass (Eleusine indica)

annual ryegrass (Lolium multiflorum)

rice (Oryza sativa)

ottochloa (Ottochloa nodosa)

bahiagrass (Paspalum notatum)

canarygrass (Phalaris spp.)

foxtail (Setaria spp.)

wheat (Triticum aestivum)

corn (Zea mays)

Perennial broadleaves:

mugwort (Artemisia spp.)

milkweed (Asclepias spp.)

canada thistle (Cirsium arvense)

field bindweed (Convolvulus arvensis)

kudzu (Pueraria spp.)

Perennial narrowleaves:

brachiaria (Brachiaria spp.)

bermudagrass (Cynodon dactylon)

yellow nutsedge (Cyperus esculentus)

purple nutsedge (C. rotundus)

quackgrass (Elymus repens)

lalang (Imperata cylindrica)

perennial ryegrass (Lolium perenne)

guineagrass (Panicum maximum)

dallisgrass (Paspalum dilatatum)

reed (Phragmites spp.)

johnsongrass (Sorghum halepense)

cattail (Typha spp.)

Other perennials:

horsetail (Equisetum spp.)

bracken (Pteridium aquilinum)

blackberry (Rubus spp.)

gorse (Ulex europaeus)

Thus, the method of the present invention, as it pertains to glyphosate herbicide, can be useful on any of the above species.

Effectiveness in greenhouse tests, usually at exogenous chemical rates lower than those normally effective in the field, is a proven indicator of consistency of field performance at normal use rates. However, even the most promising composition sometimes fails to exhibit enhanced performance in individual greenhouse tests. As illustrated in the Examples herein, a pattern of enhancement emerges over a series of greenhouse tests; when such a pattern is identified this is strong evidence of biological enhancement that will be useful in the field.

Aggregate-forming substances useful as the first excipient substance in compositions of the present invention include a wide variety of amphiphilic materials, of which three classes are preferred.

The first preferred class of aggregate-forming substances can be defined as amphiphilic liposome-forming substances. These include various lipids of synthetic, animal, or plant origin, including phospholipids, ceramides, sphingolipids, dialkyl surfactants, and polymeric surfactants. A variety of these materials are known to those skilled in the art, and are commercially available. Lecithins are particularly rich in phospholipids and can be derived from a number of plant and animal sources. Soybean lecithin is one particular example of a relatively inexpensive commercially available material that includes such substances.

Many other substances have been described which can be used to form liposomes; the present invention includes compositions comprising any such liposome-forming substances, so long as other requirements set out above are met, and use of such compositions for enhancing biological effectiveness of exogenous chemicals applied to foliage of plants. For example, U.S. Pat. No. 5,580,859, incorporated here by reference, discloses liposome-forming substances having a cationic group, including N-(2,3-di-(9-(Z)-octadecenyloxy))-prop-1-yl-N,N,N-trimethylammonium chloride (DOTMA) and 1,2-bis(oleoyloxy)-3-(trimethylammonio)propane (DOTAP). Liposome-forming substances which are not themselves cationic, but do contain a cationic group as part of the hydrophilic moiety, include for example dioleoylphosphatidylcholine (DOPC) and dioleoylphosphatidylethanolamine (DOPE). Liposome-forming substances that do not contain a cationic group include dioleoylphosphatidylglycerol (DOPG). Any of these liposome-forming substances can be used with or without the addition of cholesterol.

These substances contain portions that are hydrophilic and hydrophobic within the same molecule. They have the ability to self-assemble in aqueous solution or dispersion into structures that are more complex than simple micelles. The nature of the aggregate that will be formed can be related to the critical packing parameter P by the following equation:

    P=V/lA

where V is the volume of the hydrophobic tail of the molecule, l is the effective length of the hydrophobic tail, and A is the area occupied by the hydrophilic headgroup in the surface of the aggregate. The most probable self-assembled structures are spherical micelles when P is less than 1/3, rodlike micelles when P is between 1/3 and 1/2, lamellar when P is between 1 and 1/2, and inverse structures when P is greater than 1. The preferred materials in the present invention have P greater than 1/3.

Cationic liposome-forming substances having a hydrophobic moiety comprising two hydrocarbyl chains are accompanied by a counterion (anion), identified as Z in formulas I, II and III above. Any suitable anion can be used, including agriculturally acceptable anions such as hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate. In a specific embodiment where the exogenous chemical has a biologically active anion, that anion can serve as the counterion for the liposome-forming substance. For example, glyphosate can be used in its acid form together with the hydroxide of a cationic liposome-forming substance such as a compound of formula I.

Compounds of formula I known in the art to be liposome-forming include distearyldimethylammonium chloride and bromide (also known in the art as DODAC and DODAB respectively). Compounds of formula II known in the art to be liposome-forming include DOTMA referenced above and dimyristooxypropyldimethylhydroxyethylammonium bromide (DMRIE). Compounds of formula III known in the art to be liposome-forming include dioleoyloxy-3-(dimethylammonio)propane (DODAP) and DOTAP referenced above. Compounds of formula IV known in the art to be liposome-forming include DOPC and DOPE, both referenced above.

In many liposome-forming substances known in the art, the hydrophobic hydrocarbyl chains are unsaturated, having one or more double bonds. Particularly commonly used in the pharmaceutical art are dioleyl or dioleoyl compounds. A potential problem with these is that in an oxidizing environment they become oxidized at the site of the double bond. This can be inhibited by including in the formulation an antioxidant such as ascorbic acid. Alternatively the problem can be avoided by use of liposome-forming substances wherein a high proportion of the hydrophobic hydrocarbyl chains are fully saturated. Thus in a preferred embodiment of the invention, R¹ and R² in formulas I-IV are independently saturated straight-chain alkyl groups. Particularly preferred compositions use liposome-forming substances in which R¹ and R² are both palmityl (cetyl) or palmitoyl or, alternatively, are both stearyl or stearoyl groups.

Phospholipids, because of their low cost and favorable environmental properties, are particularly favored among liposome-forming substances in the method and compositions of the invention. Vegetable lecithins, such as soybean lecithin, have successfully been used in accordance with the invention. The phospholipid content of the lecithin product can range from about 10% to close to 100%. While acceptable results have been obtained with crude lecithin (10-20% phospholipid), it is generally preferred to use lecithin that is at least partially de-oiled, so that the phospholipid content is in the region of about 45% or more. Higher grades, such as 95%, provide excellent results but the much higher cost is unlikely to be justified for most applications.

The phospholipid component of lecithin, or any phospholipid composition used in the present invention, may comprise one or more phosphatides of natural or synthetic origin. Each of these phosphatides is generally a phosphoric ester that on hydrolysis yields phosphoric acid, fatty acid(s), polyhydric alcohol and, typically, a nitrogenous base. A phosphatide component may be present in a partially hydrolyzed form, e.g. as phosphatidic acid. Suitable phosphatides include, without limitation, phosphatidylcholine, hydrogenated phosphatidyleholine, phosphatidylinositol, phosphatidylserine, phosphatidic acid, phosphatidylglycerol, phosphatidylethanolamine, N-acyl phosphatidylethanolamine, and mixtures of any of these.

In vegetable lecithins a high proportion of the hydrophobic hydrocarbyl chains of the phospholipid compounds are typically unsaturated. One preferred embodiment of compositions in accordance with the present invention comprises both saturated phospholipid and unsaturated phospholipid, with the weight ratio of saturated phospholipid to unsaturated phospholipid being greater than about 1:2. In various particularly preferred embodiments, (1) at least 50% by weight of the phospholipids are di-C₁₂₋₂₂ -saturated alkanoyl phospholipid, (2) at least 50% by weight of the phospholipids are di-C₁₆₋₁₈ -saturated alkanoyl phospholipid, (3) at least 50% by weight of the phospholipids are distearoyl phospholipid, (4) at least 50% by weight of the phospholipids are dipalmitoyl phospholipid, or (5) at least 50% by weight of the phospholipids are distearoyl phosphatidylcholine, dipalmitoyl phosphatidylcholine, or a mixture thereof. Higher proportions of saturated alkanoyl phospholipids are generally found in lecithins of animal origin, such as for example egg yolk lecithin, than in vegetable lecithins.

Phospholipids are known to be chemically unstable, at least in acid media, where they tend to degrade to their lyso-counterparts. Thus where phospholipids rather than more stable liposome-forming substances are used, it is usually preferable to adjust the pH of the composition upward. In the case of glyphosate compositions, the pH of a composition based on a mono-salt such as the monoisopropylammonium (IPA) salt is typically around 5 or lower. When phospholipids are used as the first excipient substance in a glyphosate composition of the invention, it will therefore be preferable to raise the pH of the composition, for example to around 7. Any convenient base can be used for this purpose; it will often be most convenient to use the same base as used in the glyphosate salt, for example isopropylamine in the case of glyphosate IPA salt.

Amphiphilic compounds useful as the first excipient substance herein are not limited to those having two hydrophobic hydrocarbyl groups such as the compounds of formulas I to IV. The second preferred class of aggregate-forming substances useful in the invention are cationic surfactant compounds having formula V above. In compounds of formula V, R⁸ unless perfluorinated preferably has from about 12 to about 18 carbon atoms. R⁸ is preferably perfluorinated, in which case it preferably has from about 6 to about 12 carbon atoms. Preferably n is 3. R⁹ groups are preferably methyl.

Sulfonylamino compounds of formula V are especially preferred. Suitable examples include 3-(((heptadecafluorooctyl)sulfonyl)amino)-N,N,N-trimethyl-1-propaminium iodide, available for example as Fluorad FC-135 from 3M Company, and the corresponding chloride. It is believed that Fluorad FC-754 of 3M Company is the corresponding chloride.

Fluoro-organic surfactants such as the cationic types falling within formula V belong to a functional category of surfactants known in the art as "superspreaders" or "superwetters". As a class "superspreaders" or "superwetters" are very effective in reducing surface tension of aqueous compositions containing relatively low concentrations of these surfactants. In many applications fluoro-organic surfactants can substitute for organosilicone surfactants which are likewise "superspreaders" or "superwetters". An example is found in European patent application 0 394 211 which discloses that either organosilicone or fluoro-organic surfactants can be used interchangeably in solid granular formulations of pesticides to improve dissolution rate.

Two major problems have limited interest in "superspreaders" and "superwetters" by formulators of exogenous chemicals such as pesticides. The first is high unit cost. The second is that although surfactants of this functional category can enhance performance of an exogenous chemical on some species, for example by assisting penetration of the exogenous chemical into the interior of leaves via stomata, they can be antagonistic, sometimes severely so, to performance of the same exogenous chemical on other species.

Surprisingly, a subclass of fluoro-organic surfactants has now been found to be essentially non-antagonistic at concentrations which nevertheless provide useful adjuvant effects. This subclass comprises cationic fluoro-organic surfactants of formula V and others having a property profile in common with those of formula V. The lack of antagonism makes this subclass very different from other fluoro-organic "superspreaders" or "superwetters". Further, it has been found that these non-antagonistic fluoro-organic surfactants can be useful at concentrations low enough to be cost-effective. Data in the Examples herein for compositions comprising Fluorad FC-135 or Fluorad FC-754 illustrate the unexpected properties of this subclass.

Derivatives of Fluorad FC-754, herein described as "FC-acetate" and "FC-salicylate," have been prepared by the following procedure. (I) The solvent in a sample of Fluorad FC-754 is gently evaporated off by heating in a glass beaker at 70-80° C., to leave a solid residue. (2) The solid residue is allowed to cool to room temperature. (3) A 1 g aliquot of the residue is placed in a centrifuge tube and dissolved in 5 ml isopropanol. (4) A saturated solution of potassium hydroxide (KOH) is prepared in isopropanol. (5) This solution is added drop by drop to the solution of FC-754 residue; this results in formation of a precipitate and addition of KOH solution continues until no further precipitate forms. (6) The tube is centrifuged at 4000 rpm for 5 minutes. (7) More KOH solution is added to check if precipitation is complete; if not, the tube is centrifuged again. (8) The supernatant is decanted into another glass tube. (9) A saturated solution of acetic acid (or salicylic acid) is prepared in isopropanol. (10) This solution is added to the supernatant in an amount sufficient to lower pH to 7. (11) Isopropanol is evaporated from this neutralized solution by heating at 60° C. until completely dry. (12) The residue (either the acetate or salicylate salt) is dissolved in a suitable amount of water and is then ready for use.

The third preferred class of aggregate-forming substance useful as the first excipient substance according to the present invention is a long-chain alkylether surfactant having the formula VI above. R¹² can be branched or unbranched, saturated or unsaturated. R¹² is preferably straight chain saturated C₁₆ alkyl (cetyl) or straight chain saturated C₁₋₈ alkyl (stearyl). In preferred alkylethers m is 0, n is an average number from about 20 to about 40 and R¹³ is preferably hydrogen. Among especially preferred alkylether surfactants are those identified in the International Cosmetic Ingredient Directory as ceteth-20, ceteareth-20, ceteareth-27, steareth-20 and steareth-30.

Of the classes of aggregate-forming substance useful as the first excipient substance, not all give rise to anisotropic aggregates in or on a wax layer, as required by the present invention, when used as the sole excipient substance in the composition at a weight ratio of 1:3 to 1:100 with the exogenous chemical. Many compounds of formulas V and VI are sufficient in the absence of a second excipient substance, but in general the liposome-forming substances of formulas I to IV require the presence of a second excipient substance to exhibit the required anisotropic behavior. However, even in the presence of a first excipient substance of formulas V or VI, there may be advantages in also including a second excipient substance as herein defined.

The second excipient substance has one or more hydrophobic moieties. If there is only one hydrophobic moiety, it is a hydrocarbyl or haloalkyl group having about 6 to about 22 carbon atoms. If there is more than one hydrophobic moiety, each such moiety is a hydrocarbyl or haloalkyl group having more than 2 carbon atoms, and the total number of carbon atoms in the hydrophobic moieties is about 12 to about 40.

One class of second excipient substance useful in the present invention is quaternary ammonium compounds. Among quaternary ammonium compounds that may be used are compounds of formula

    N.sup.+ (R.sup.16)(R.sup.17)(R.sup.18)(R.sup.19)Q.sup.-    VIII

where R¹⁶, R¹⁷, R¹⁸ and R¹⁹ are independently C₃₋₆ alkyl groups and Q is a suitable anion, such as for example hydroxide, chloride, bromide, iodide, sulfate, phosphate or acetate. In preferred compounds of formula VIII all R groups are the same. Particularly preferred compounds of formula VIII are tetrabutylammonium salts. Where the exogenous chemical comprises a biologically active anion, a salt of formula VIII where Q is that anion is an option providing both the exogenous chemical and second excipient substance. An example is the tetrabutylammonium salt of glyphosate.

Other quaternary ammonium compounds that may be useful include compounds having a single C₁₂₋₂₂ hydrocarbyl group and three C₁₋₄ alkyl groups attached to the quaternary nitrogen atom. One or more of the C₁₋₄ alkyl groups in such compounds can be replaced by a benzyl group. Specific examples include cetyltrimethylammonium bromide and benzalkonium chloride. Yet other quaternary ammonium compounds useful as the second excipient substance include compounds of formula I, where the first excipient substance is not of formula I.

Preferred quaternary ammonium compounds useful as the second excipient substance are compounds of formula V, where the first excipient substance is not of formula V. The same specific compounds of formula V are especially preferred whether a compound of formula V is the first or the second excipient substance. Particularly good results have been obtained where the first excipient substance is lecithin and the second excipient substance is Fluorad FC-135 or FC-754 or chemical equivalents thereof.

Another class of compound useful as the second excipient substance is an amide or ester of formula VII above.

R¹⁴ in formula VII is preferably aliphatic and has about 7 to about 21 carbon atoms, more preferably about 13 to about 21 carbon atoms. It is especially preferred that R¹⁴ be a saturated straight-chain alkyl group. R¹⁵ is preferably an aliphatic group having 1-6 carbon atoms, more preferably alkyl or alkenyl having 2-4 carbon atoms. An especially preferred compound of formula VII for use as the second excipient substance is butyl stearate.

As compounds of formula VII, including butyl stearate, are generally oily liquids, aqueous compositions containing them are typically emulsions having at least one aqueous phase and at least one oil phase, with the compound of formula VII being present predominantly in the oil phase. Such emulsions may be water-in-oil, oil-in-water or water-in-oil-in-water (W/O/W) multiple emulsions.

Aqueous concentrate compositions where the first excipient substance is an alkylether of formula VI and the second excipient substance, if present, is a fatty acid ester of formula VII are limited in the degree to which an exogenous chemical such as glyphosate can be loaded. At some point, as the loading of exogenous chemical is increased, the composition will not remain suitably stable. Addition of a small amount of colloidal particulate to such compositions has surprisingly been found to greatly increase loading ability while retaining desired stability. Oxides of silicon, aluminum and titanium are preferred colloidal particulate materials. Particle size is preferably such that specific surface area is in the range from about 50 to about 400 m² /g. Where the exogenous chemical is glyphosate, the use of colloidal particulate enables loadings of at least 30% by weight for compositions containing sufficient alkylether and fatty acid ester to show enhanced herbicidal effectiveness, or at least 40% for compositions containing alkylether but no fatty acid ester, and showing herbicidal effectiveness at least equal to current commercial products loaded at about 30%. We have found especially useful improvement in storage stability can be obtained using colloidal particulates having specific surface area between about 180 and about 400 m² /g.

Other means of improving stability of highly loaded compositions comprising an alkylether of formula VI, with or without a fatty acid ester, may also be possible and are within the scope of the present invention.

Compositions in accordance with the present invention are typically prepared by combining water, the exogenous chemical (unless it is a formulation which will not contain an exogenous chemical) and the aggregate-forming substance. Where the aggregate-forming substance is one that disperses readily in water, as is the case for example with Fluorad FC-135 or Fluorad FC-754, simple mixing with mild agitation may be sufficient. However, where the aggregate-forming substance requires high shear to disperse in water, as is the case for example with most forms of lecithin, it is presently preferred to sonicate or microfluidize the aggregate-forming substance in water. This can be done before or after a surfactant and/or the exogenous chemical is added. The sonication or microfluidization will generally produce liposomes or other aggregate structures other than simple micelles. The precise nature, including average size, of liposomes or other aggregates depends among other things on the energy input during sonication or microfluidization. Higher energy input generally results in smaller liposomes. Although it is possible to entrap or otherwise bind loosely or tightly the exogenous chemical in or on liposomes or with other supramolecular aggregates, the exogenous chemical does not need to be so entrapped or bound, and in fact the present invention is effective when the exogenous chemical is not entrapped or bound in the aggregates at all.

In a particular embodiment of the invention, the liposomes or other aggregates have an average diameter of at least 20 nm, more preferably at least 30 nm. We have determined by light scattering that certain liposomal compositions of the invention have average liposome diameters ranging from 54 to 468 nm as calculated using linear fit and from 38 to 390 nm as calculated using quadratic fit.

The concentrations of the various components will vary, in part depending on whether a concentrate is being prepared that will be further diluted before spraying onto a plant, or whether a solution or dispersion is being prepared that can be sprayed without further dilution.

In an aqueous glyphosate formulation that includes a dialkyl surfactant, for example a cationic dialkyl surfactant of formula I, suitable concentration ranges are: glyphosate 0.1-400 grams acid equivalent (a.e.)/liter, and dialkyl surfactant 0.001-10% by weight. In an aqueous glyphosate formulation using a cationic fluoro-organic surfactant and lecithin, suitable concentrations can be: glyphosate 0.1-400 g a.e./l, fluoro-organic surfactant 0.001-10% by weight, and soybean lecithin 0.001-10% by weight.

In an aqueous glyphosate formulation that includes a C₁₆₋₁₈ alkylether surfactant and butyl stearate, suitable concentrations can be: glyphosate 0.1-400 g a.e./l, alkylether surfactant 0.001-10% by weight, and butyl stearate 0.001-10% by weight. To achieve the higher concentrations in these ranges, it is often beneficial to add other ingredients to provide acceptable storage stability, for example colloidal particulate silica or aluminum oxide at 0.5-2.5% by weight. In an aqueous glyphosate formulation that includes a C₁₆₋₁₈ alkylether surfactant but no butyl stearate, glyphosate concentration can suitably be increased to 500 g a.e./l or more, in the presence of a colloidal particulate at 0.5-2.5% by weight.

In solid glyphosate formulations, higher concentrations of ingredients are possible because of the elimination of most of the water.

Weight/weight ratios of ingredients may be more important than absolute concentrations. For example, in a glyphosate formulation containing lecithin and a cationic fluoro-organic surfactant, the ratio of lecithin to glyphosate a.e. is in the range from about 1:3 to about 1:100. It is generally preferred to use a ratio of lecithin to glyphosate a.e. close to as high as can be incorporated in the formulation while maintaining stability, in the presence of an amount of the fluoro-organic surfactant sufficient to give the desired enhancement of herbicidal effectiveness. For example, a lecithin/glyphosate a.e. ratio in the range from about 1:3 to about 1:10 will generally be found useful, although lower ratios, from about 1:10 to about 1:100 can have benefits on particular weed species in particular situations. The ratio of fluoro-organic surfactant, when present, to glyphosate a.e. is likewise preferably in the range from about 1:3 to about 1:100. Because fluoro-organic surfactants tend to have relatively high cost, it will generally be desirable to keep this ratio as low as possible consistent with achieving the desired herbicidal effectiveness.

The ratio of fluoro-organic surfactant, where present, to lecithin is preferably in the range from about 1:10 to about 10:1, more preferably in the range from about 1:3 to about 3:1 and most preferably around 1:1. The ranges disclosed herein can be used by one of skill in the art to prepare compositions of the invention having suitable concentrations and ratios of ingredients. Preferred or optimum concentrations and ratios of ingredients for any particular use or situation can be determined by routine experimentation.

Although the combination of the components might be done in a tank mix, it is preferred in the present invention that the combination be made further in advance of the application to the plant, in order to simplify the tasks required of the person who applies the material to plants. We have found, however, that in some cases the biological effectiveness of a liposome-containing composition prepared from scratch as a dilute spray composition is superior to that of a composition having the same ingredients at the same concentrations but diluted from a previously prepared concentrate formulation.

Although various compositions of the present invention are described herein as comprising certain listed materials, in some preferred embodiments of the invention the compositions consist essentially of the indicated materials.

Optionally, other agriculturally acceptable materials can be included in the compositions. For example, more than one exogenous chemical can be included. Also, various agriculturally acceptable adjuvants can be included, whether or not their purpose is to directly contribute to the effect of the exogenous chemical on a plant. For example, when the exogenous chemical is a herbicide, liquid nitrogen fertilizer or ammonium sulfate might be included in the composition. As another example, stabilizers can be added to the composition. In some instances it might be desirable to include microencapsulated acid in the composition, to lower the pH of a spray solution on contact with a leaf. One or more surfactants can also be included. Surfactants mentioned here by trade name, and other surfactants that can be useful in the method of the invention, are indexed in standard reference works such as McCutcheon's Emulsifiers and Detergents, 1997 edition, Handbook of Industrial Surfactants, 2nd Edition, 1997, published by Gower, and International Cosmetic Ingredient Dictionary, 6th Edition, 1995.

The compositions of the present invention can be applied to plants by spraying, using any conventional means for spraying liquids, such as spray nozzles, atomizers, or the like. Compositions of the present invention can be used in precision farming techniques, in which apparatus is employed to vary the amount of exogenous chemical applied to different parts of a field, depending on variables such as the particular plant species present, soil composition, and the like. In one embodiment of such techniques, a global positioning system operated with the spraying apparatus can be used to apply the desired amount of the composition to different parts of a field.

The composition at the time of application to plants is preferably dilute enough to be readily sprayed using standard agricultural spray equipment. Preferred application rates for the present invention vary depending upon a number of factors, including the type and concentration of active ingredient and the plant species involved. Useful rates for applying an aqueous composition to a field of foliage can range from about 25 to about 1,000 liters per hectare (l/ha) by spray application. The preferred application rates for aqueous solutions are in the range from about 50 to about 300 l/ha.

Many exogenous chemicals (including glyphosate herbicide) must be taken up by living tissues of the plant and translocated within the plant in order to produce the desired biological (e.g., herbicidal) effect. Thus, it is important that a herbicidal composition not be applied in such a manner as to excessively injure and interrupt the normal functioning of the local tissue of the plant so quickly that translocation is reduced. However, some limited degree of local injury can be insignificant, or even beneficial, in its impact on the biological effectiveness of certain exogenous chemicals.

A large number of compositions of the invention are illustrated in the Examples that follow. Many concentrate compositions of glyphosate have provided sufficient herbicidal effectiveness in greenhouse tests to warrant field testing on a wide variety of weed species under a variety of application conditions. Water-in-oil-in-water multiple emulsion compositions tested in the field have included:

    __________________________________________________________________________                 % w/w                                                                          Fatty                             Type of                            Field Glyphosate acid Emulsifier Emulsifier % in inner aq. phase                                                           Emulsifier Emulsifier fatty                                                    acid                             composition                                                                          g a.e./l                                                                             ester                                                                              #1   #2   Water                                                                              Glyphosate                                                                           #1   #2   ester                            __________________________________________________________________________     F-1   100   18.0                                                                               3.0  5.0  13.8                                                                               20    Span 80                                                                             Tween 20                                                                            Bu stearate                        F-2 100 7.5 3.0 5.0 5.6 20 Span 80 Tween 20 Bu stearate                        F-3 100 7.5 3.0 5.0 5.6  0 Span 80 Tween 20 Bu stearate                        F-4 160 7.5 3.0 5.0 5.6  0 Span 80 Tween 20 Bu stearate                      __________________________________________________________________________

The above compositions were prepared by process (vi) as described in the Examples.

Aqueous compositions tested in the field having an alkylether surfactant as the first excipient substance and/or containing a fatty acid ester have included:

    ______________________________________                                                 % w/w                                                                  Field Gly-    Fatty                   Type                                       compo- phosate acid Sur- Type of of fatty                                      sition g a.e./l ester factant surfactant acid ester                          ______________________________________                                         F-5   163     1.0    10.0   oleth-20  Bu stearate                                F-6  163 1.0 10.0  Tween 80 Bu stearate                                        F-7  163 1.0 10.0  Neodol 25-20 Bu stearate                                    F-8  163 1.0 10.0  steareth-20 Bu stearate                                     F-9  163 1.0 10.0  Neodol 25-12 Bu stearate                                    F-10 105 7.5 10.0  Tween 80 Bu stearate                                        F-11 163 0.5 5.0 oleth-20 Bu stearate                                          F-12 163 0.3 5.0 oleth-20 Bu stearate                                          F-13 163 0.3 2.5 oleth-20 Bu stearate                                          F-14 163 1.0 10.0  Neodol 25-12 Bu stearate                                    F-15 163 0.3 5.0 Genapol UD-110 Bu stearate                                    F-16 163 0.5 5.0 steareth-20 Bu stearate                                       F-17 163 0.5 5.0 ceteth-20 Bu stearate                                         F-18 163 0.5 5.0 laureth-23 Bu stearate                                        F-19 163 0.5 5.0 ceteareth-27 Bu stearate                                      F-20 163 0.5 5.0 Neodol 25-12 Bu stearate                                      F-21 163 0.5 5.0 Neodol 25-20 Bu stearate                                      F-22 163  5.0 steareth-20                                                      F-23 163  5.0 ceteth-20                                                        F-24 163  5.0 laureth-23                                                       F-25 163 0.3 5.0 ceteareth-27 Bu stearate                                      F-26 163 0.3 2.5 ceteareth-27 Bu stearate                                      F-27 163  5.0 ceteareth-27                                                     F-28 163 0.5 5.0 ceteareth-27 Me stearate                                      F-29 163 0.5 5.0 steareth-20 Me stearate                                       F-30 163 0.5 5.0 oleth-20                                                      F-31 163 0.5 5.0 Neodol 45-13 Bu stearate                                      F-32 163  5.0 Neodol 45-13                                                     F-33 163 0.5 5.0 ceteareth-15 Bu stearate                                      F-34 163  5.0 ceteareth-15                                                     F-35 163 0.5 5.0 steareth-30 Bu stearate                                     ______________________________________                                    

The above compositions were prepared by process (vii) if they contain fatty acid ester and by process (viii) if they do not. Both processes are described in the Examples.

Aqueous compositions tested in the field containing colloidal particulates have included:

    __________________________________________________________________________                 % w/w                                                                          Fatty                 Type of                                                                               Type of                                 Field Glyphosate acid Sur- Coll.  Type of colloidal fatty acid Other                                                         composition g a.e./l                                                          ester factant partic.                                                          Other surfactant particulat                                                    e ester ingredients             __________________________________________________________________________     F-36  360   1.0 10.0                                                                               1.3     steareth-20                                                                          Aerosil 380                                                                           Bu stearate                             F-37 360 1.0 10.0 1.3  oleth-20 Aerosil 380 Bu stearate                        F-38 360 1.0 10.0 1.3  steareth-30 Aerosil 380 Bu stearate                     F-39 360  10.0 1.3  steareth-30 Aerosil 380                                    F-40 360   0.8   Aerosil 90                                                    F-41 350   0.8   Al oxide C                                                    F-42 360  3.0 0.8  Ethomeen Al oxide C                                               T/25                                                                     F-43 360  3.0 0.1  Ethomeen Al oxide C                                               T/25                                                                     F-44 360   0.3   Al oxide C                                                    F-45 360  3.0 0.3  Ethomeen Al oxide C                                               T/25                                                                     F-46 360  6.0 0.8  Agrimul Al oxide C                                                PG-2069                                                                  F-47 360  3.0 0.8  Tween 20 Al oxide C                                         F-48 480  1.0 0.4  Neodol 1-7 Aerosil 90                                       F-49 480  2.0 0.4  Agrimul Aerosil 90                                                PG-2069                                                                  F-50 360 1.0 10.0 1.3  ceteareth- Aerosil 380 Bu stearate                            15                                                                       F-51 360 1.0 10.0 1.3  ceteth-20 Aerosil 380 Bu stearate                       F-52 360 1.0 10.0 1.3  steareth-20 Aerosil 380 Bu stearate                     F-53 360 1.0 10.0 1.3  oleth-20 Aerosil 380 Bu stearate                        F-54 360 1.0 10.0 1.3  ceteareth- Aerosil 380 Bu stearate                            27                                                                       F-55 360 1.0 10.0 1.3  steareth-30 Aerosil 380 Bu stearate                     F-56 360  10.0 1.3  steareth-30 Aerosil 380                                    F-57 360  10.0 1.3  ceteareth- Aerosil 380                                           27                                                                       F-58 360  10.0 1.3  steareth-20 Aerosil 380                                    F-59 360  10.0 1.3  oleth-20 Aerosil 380                                       F-60 360 1.0 10.0 1.3  ceteareth- Aerosil 380 Me stearate                            27                                                                       F-61 360 1.0 10.0 1.3  ceteareth- Aerosil 380 Me palmitate                           27                                                                       F-62 300  10.0 1.3  ceteareth- Aerosil 380                                           27                                                                       F-63 240  10.0 1.3  ceteareth- Aerosil 380                                           27                                                                       F-64 360  6.0 1.3  ceteareth- Aerosil 380                                            27                                                                       F-65 300  6.0 1.3  ceteareth- Aerosil 380                                            27                                                                       F-66 240  6.0 1.3  ceteareth- Aerosil 380                                            27                                                                       F-67 360   0.6   Aerosil 90                                                    F-68 360   3.1   Aerosil 90                                                    F-69 360   0.6   Al oxide C                                                    F-70 360   3.1   Al oxide C                                                    F-71 360   0.8   Aerosil 90                                                    F-72 360   0.8   Al oxide C                                                    F-73 360  3.0 0.8  Ethomeen Aerosil 90                                               T/25                                                                     F-74 360  3.0 0.8  Ethomeen Al oxide C                                               T/25                                                                     F-75 360  3.0 0.3  Ethomeen Al oxide C                                               T/25                                                                     F-76 360  3.0 0.8  Ethomeen Nalco 1056                                               T/25                                                                     F-77 360  3.0 0.8  Ethomeen Nalco 1056                                               C/25                                                                     F-78 480  3.0 +  0.4  Ethomeen Al oxide C                                         1.0   T/25 +                                                                      Agrimul                                                                        PG-2069                                                                  F-79 480  3.0 + 0.4  Ethomeen Al oxide C                                          3.0   T/25 +                                                                      Agrimul                                                                        PG-2069                                                                  F-80 360  3.0 0.8  Agrimul Aerosil 90                                                PG-2069                                                                  F-81 360  3.0 0.8  Tween 20 Aerosil 90                                         F-82 360  3.1 + 0.8 7.1 Ethomeen Aerosil 90  (Bu).sub.4 NOH                       3.1   T/25 +                                                                      Tween 20                                                                 F-83 360   0.8 7.1  Aerosil 90  (Bu).sub.4 NOH                                 F-84 480  3.0 0.8  steareth-20 Aerosil 380                                     F-85 480  3.0 1.5  oleth-20 Aerosil 380                                        F-86 480  3.0 1.5  oleth-20 Aerosil                                                   MOX-170                                                                 F-87 480  3.0 1.5  oleth-20 Aerosil                                                   OX-50                                                                   F-88 480  3.0 1.5  Velvetex Aerosil 380                                              AB-45                                                                    F-89 480  3.0 1.5  steareth-20 Aerosil blend                                          2                                                                       F-90 480  3.0 1.5  oleth-20 Aerosil blend                                             2                                                                       F-91 480  4.5 1.5  oleth-20 Aerosil 380                                        F-92 480  4.5 1.5  steareth-20 Aerosil 380                                     F-93 480  3.0 1.5  steareth-20 Aerosil blend                                          1                                                                       F-94 480  1.0 1.5  steareth-20 Aerosil blend                                          1                                                                       F-95 480  6.0 1.5  steareth-20 Aerosil blend                                          1                                                                       F-96 480  4.5 1.5 0.5 steareth-20 Aerosil blend  propylene                            2  glycol                                                               F-97 480  6.0 1.5 0.5 steareth-20 Aerosil blend  propylene                            2  glycol                                                               F-98 480  6.0 1.5 0.5 oleth-20 Aerosil blend  propylene                              2  glycol                                                                F-99 480  4.5 + 1.5 0.5 steareth-20 Aerosil blend  propylene                      2.3   + 2  glycol                                                                 Ethomeen                                                                       T/25                                                                     F-100 480  6.0 1.5  steareth-20 Al oxide C                                     F-101 480  4.5 + 1.5 0.5 steareth-20 Al oxide C  propylene                        2.3   +   glycol                                                                  Ethomeen                                                                       T/25                                                                     F-102 480  4.5 + 1.5 0.5 steareth-20 Al oxide C  propylene                        1.0   +   glycol                                                                  Ethomeen                                                                       T/25                                                                     F-103 480  3.0 1.5  steareth-20 Aerosil 380                                    F-104 480  4.5 1.5  steareth-20 Al oxide C                                     F-105 480  6.0 1.5  steareth-20 Aerosil 380                                    F-106 480  4.5 + 1.5 0.5 steareth-20 Aerosil 380  propylene                       1.0   +   glycol                                                                  Ethomeen                                                                        T/25                                                                    F-107 480  4.5 + 1.5 0.5 steareth-20 Aerosil 380  propylene                       2.3   +   glycol                                                                  Ethomeen                                                                       T/25                                                                     F-108 480  4.5 1.5  steareth-20 Aerosil blend                                         2                                                                       F-109 480  6.0 1.5  steareth-20 Aerosil blend                                         2                                                                       F-110 480  4.5 + 1.5 0.5 steareth-20 Aerosil blend  propylene                     1.0   + 2  glycol                                                                 Ethomeen                                                                       T/25                                                                     F-111 480  4.5 1.5  steareth-30 Aerosil blend                                         2                                                                       F-112 480  4.5 + 1.5 0.5 steareth-20 Aerosil blend  propylene                     1.0   + 2  glycol                                                                 Ethomeen                                                                       T/25                                                                     F-113 480  6.0 1.5  steareth-30 Aerosil blend                                         2                                                                       F-114 480  4.5 + 1.5 0.5 steareth-20 Aerosil blend  propylene                     2.3   + 2  glycol                                                                 Ethomeen                                                                       T/25                                                                     F-115 480  10.0 1.5  steareth-20 Aerosil blend                                        2                                                                       F-116 480  4.5 1.5  ceteareth- Aerosil 380                                           27                                                                       F-117 480  6.0 1.5  ceteareth- Aerosil 380                                           27                                                                       F-118 480  4.5 1.5  ceteareth- Aerosil blend                                         27 2                                                                     F-119 480  6.0 1.5  ceteareth- Aerosil blend                                         27 2                                                                     F-120 480  4.5 1.5  ceteareth- Al oxide C                                            27                                                                       F-121 480  6.0 1.5  ceteareth- Al oxide C                                            27                                                                     __________________________________________________________________________      Aerosil blend 1: Aerosil MOX80 + Aerosil MOX170 (1:1)                          Aerosil blend 2: Aerosil MOX80 + Aerosil 380 (1:2)                       

The above compositions were prepared by process (ix) as described in the Examples.

Aqueous compositions tested in the field having soybean lecithin (45% phospholipid, Avanti) as the first excipient substance and fatty acid ester as the second excipient substance have included:

    ______________________________________                                                      % w/w                                                             Field   Glyphosate         Fluorad                                                                               Fluorad                                                                              MON                                      composition g a.e./l Lecithin FC-135 FC-754 0818                             ______________________________________                                         F-122   167        6.0     8.3          4.0                                      F-123 168 6.0  8.3 4.0                                                         F-124 228 2.0  2.0 0.5                                                         F-125 347 3.0  3.0 0.5                                                         F-126 344 1.0  1.0 0.5                                                         F-127 111 8.0 8.0  0.5                                                         F-128 228 6.0  3.0 6.0                                                         F-129 228 6.0  6.0 6.0                                                         F-130 228 3.3  5.0 0.5                                                         F-131 228 5.0  5.0 0.8                                                         F-132 372 3.0  3.0 0.8                                                         F-133 372 3.0  5.0 0.8                                                         F-134 372 3.0  12.0   0.8                                                    ______________________________________                                    

The above compositions were prepared by process (v) as described in the Examples.

Aqueous compositions tested in the field having soybean lecithin (45% phospholipid, Avanti) as the first excipient substance and fatty acid ester as the second excipient substance have included:

    __________________________________________________________________________                 % w/w                                                              Field Glyphosate                                                                               MON                                                                               Fatty acid                                                                               Type of                                                                               Type of                                      composition g a.e./l Lecithin 0818 ester Surfactant surfactant fatty                                             acid ester                                 __________________________________________________________________________     F-135 360   0.5 6.0                                                                               7.5  6.0  Ethomeen T/25                                                                         Bu stearate                                  F-136 360 6.0 4.5 1.5 3.0 + 4.5 ceteareth-27 + Bu stearate                           Ethomeen T/25                                                            F-137 228 6.0 3.0 1.5 3.0 Ethomeen T/25 Bu stearate                            F-138 228 0.8  3.8 3.0 + 3.0 ceteareth-27 + Bu stearate                              Ethomeen T/25                                                            F-139 228 1.5  1.5 3.0 + 3.0 ceteareth-27 + Bu stearate                              Ethomeen T/25                                                            F-140 228 6.7 0.8 0.7 0.8 Ethomeen T/25 Bu stearate                            F-141 228 6.7 1.7 0.7 1.7 Ethomeen T/25 Bu stearate                            F-142 228 6.7 3.3 0.7 3.3 Ethomeen T/25 Bu stearate                            F-143 228 3.3 0.8 0.7 0.8 Ethomeen T/25 Bu stearate                            F-144 228 3.3 1.7 0.7 1.7 Ethomeen T/25 Bu stearate                            F-145 228 3.3 2.5 0.7 2.5 Ethomeen T/25 Bu stearate                            F-146 228 3.3 3.3 0.7 3.3 Ethomeen T/25 Bu stearate                            F-147 228 6.7 2.5 0.7 2.5 Ethomeen T/25 Bu stearate                            F-148 228  3.0 0.5 3.0 Ethomeen T/25 Bu stearate                               F-149 228 2.0 2.5 0.5 2.5 Ethomeen T/25 Bu stearate                            F-150 228 4.0 6.0 0.5   Bu stearate                                            F-151 228 4.0 6.0 2.0   Bu stearate                                            F-152 228 4.0 6.0 1.0   Bu stearate                                            F-153 228 2.0 2.0 0.5   Bu stearate                                            F-154 228 2.0 4.0 0.5   Bu stearate                                            F-155 228  6.0 0.5   Bu stearate                                             __________________________________________________________________________

The above compositions were prepared by process (x) as described in the Examples.

Dry compositions tested in the field have included:

    __________________________________________________________________________     % w/w                                 Type of                                  Field Glyphosate                                                                               Butyl                                                                              Surfac-                                                                            Coll.   Type of                                                                              colloidal                                                                            Other                                composition a.e. Lecithin stearate tant partic. Other surfactant                                                         particulate ingredients            __________________________________________________________________________     F-156 64            25.0                                                                               2.0     steareth-20                                                                          Aerosil                                            blend 1                                                                F-157 68   20.0 2.0  steareth-20 Aerosil                                               blend 1                                                                F-158 72   15.0 2.0  steareth-20 Aerosil                                               blend 1                                                                F-159 64   25.0 1.0  ceteth-20 Aerosil 380                                     F-160 65   25.0 1.0  steareth-20 Aerosil 380                                   F-161 65   25.0 1.0  oleth-20 Aerosil 380                                      F-162 67 10.0  10.0 +  1.0  Fluorad Aerosil 380                                    1.5   FC-754 +                                                                    Ethomeen                                                                       T/25                                                                    F-163 73  7.0  7.0 + 1.0  Fluorad Aerosil 380                                      1.5   FC-754 +                                                                    Ethomeen                                                                       T/25                                                                    F-164 64 12.0 3.0 12.0   MON 0818                                              F-165 64  6.7 6.7 13.2   MON 0818                                              F-166 68   20.0 2.0  steareth-20 Aerosil                                               blend 1                                                                F-167 66  2.0 20.0 2.0  steareth-20 Aerosil                                            blend 1                                                                F-168 68   20.0 2.0  oleth-20 Aerosil                                                  blend 1                                                                F-169 66  2.0 20.0 2.0  oleth-20 Aerosil                                               blend 1                                                                F-170 66  2.0 20.0 2.0  ceteareth-27 Aerosil                                           blend 1                                                                F-171 48   14.1  36.1 ceteareth-27  NH.sub.4                                            phosphate                                                             F-172 65   20.0  5.0 ceteareth-27  Na acetate                                  F-173 70   20.0   ceteareth-27                                               __________________________________________________________________________      Aerosil blend 1: Aerosil MOX80 + Aerosil MOX170 (1:1)                    

The above compositions were prepared by the process described for dry granular compositions in the Examples.

EXAMPLES

In the following Examples illustrative of the invention, greenhouse tests were conducted to evaluate relative herbicidal effectiveness of glyphosate compositions. Compositions included for comparative purposes included the following:

Formulation B: which consists of 41% by weight of glyphosate IPA salt in aqueous solution. This formulation is sold in the USA by Monsanto Company under the ACCORD® trademark.

Formulation C: which consists of 41% by weight of glyphosate IPA salt in aqueous solution with a coformulant (15% by weight) of a surfactant (MON 0818 of Monsanto Company) based on polyoxyethylene (15) tallowamine. This formulation is sold in Canada by Monsanto Company under the ROUNDUP® trademark.

Formulation J: which consists of 41% by weight of glyphosate IPA salt in aqueous solution, together with surfactant. This formulation is sold in the USA by Monsanto Company under the ROUNDUP® ULTRA trademark.

Formulation K: which consists of 75% by weight of glyphosate ammonium salt together with surfactant, as a water-soluble dry granular formulation. This formulation is sold in Australia by Monsanto Company under the ROUNDUP® DRY trademark.

Formulations B, C and J contain 356 grams of glyphosate acid equivalent per liter (g a.e./l). Formulation K contains 680 grams of glyphosate acid equivalent per kilogram (g a.e./kg).

Various proprietary excipients were used in compositions of the Examples. They may be identified as follows:

    __________________________________________________________________________     Trade name                                                                               Manufacturer                                                                          Chemical description                                          __________________________________________________________________________     Aerosil 90                                                                               Degussa                                                                               amorphous silica, 90 m.sup.2 /g                                 Aerosil 200 Degussa amorphous silica, 200 m.sup.2 /g                           Aerosil 380 Degussa amorphous silica, 380 m.sup.2 /g                           Aerosil MOX-80 Degussa amorphous silica/aluminum oxide, 80 m.sup.2 /gm                         Aerosil MOX-170 Degussa amorphous silica/aluminum                             oxide, 170 m.sup.2 /g                                           Aerosil OX-50 Degussa amorphous silica, 50 m.sup.2 /g                          Aerosil R-202 Degussa amorphous hydrophobic silica (dimethylsiloxane                          surface group)                                                  Aerosil R-805 Degussa amorphous hydrophobic silica (octyl surface                             group)                                                          Aerosil R-812 Degussa amorphous hydrophobic silica (trimethylsilyl                            surface group)                                                  Aerosol OS Cytec diisopropyl naphthalene sulfonate, Na salt                    Aerosol OT Cytec dioctyl sulfosuccinate, Na salt                               Agrimer AL-25 ISP 1-ethenyl hexadecyl-2-pyrrolidinone                          Agrimer AL-30 ISP 1-ethenyl-2-pyrrolidinone polymer                            Agrimul PG-2069 Henkel C.sub.9-11 alkylpolyglycoside                           Alcodet 218 Rhone-Poulenc isolauryl 10EO thioether                             Aluminum oxide C Degussa aluminum oxide, 100 m.sup.2 /g                        Amidox L-5 Stepan lauramide 5EO                                                Ammonyx CO Stepan palmitamine oxide                                            Ammonyx LO Stepan lauramine oxide                                              Arcosolve DPM Arco dipropyleneglycol monomethyl ether                          Diacid 1550 Westvaco cyclocarboxypropyl oleic acid                             Dowanol PNB Dow propylene glycol n-butyl ether                                 Dowanol TPNB Dow tripropylene glycol n-butyl ether                             Emerest 2421 Henkel glyceryl oleate                                            Emerest 2661 Henkel PEG-12 laurate                                             Emid 6545 Henkel oleic diethanolamide                                          Emphos CS-121 Witco alkylaryl ethoxylate phosphate ester                       Emphos CS-131 Witco alkylaryl ethoxylate phosphate ester                       Emphos CS-141 Witco nonylphenol 10EO phosphate                                 Emphos CS-330 Witco alkylaryl ethoxylate phosphate ester                       Emphos PS-21A Witco alcohol ethoxylate phosphate ester                         Emphos PS-121 Witco linear alcohol ethoxylate phosphate ester, acid                           form                                                            Emphos PS-400 Witco linear alcohol ethoxylate phosphate ester, acid                           form                                                            Ethomeen C/12 Akzo cocoamine 2EO                                               Ethomeen C/25 Akzo cocoamine 15EO                                              Ethomeen T/12 Akzo tallowamine 2EO                                             Ethomeen T/25 Akzo tallowamine 15EO                                            Ethoquad T/20 Akzo methyltallowammonium chloride 10EO                          Exxate 700 Exxon C.sub.7 alkyl acetate                                         Exxate 1000 Exxon C.sub.10 alkyl acetate                                       Exxol D-130 Exxon dearomatized aliphatic solvent                               Fluorad FC-120 3M C.sub.9-10 perfluoroalkyl sulfonate, NH4 salt                                Fluorad FC-129 3M fluorinated alkyl carboxylate, K salt        Fluorad FC-135 3M fluorinated alkyl quaternary ammonium iodide                 Fluorad FC-170C 3M fluorinated alkanol EO                                      Fluorad FC-171 3M fluorinated alkanol EO                                       Fluorad FC-431 3M fluorinated alkyl ester                                      Fluorad FC-750 3M fluorinated alkyl quaternary ammonium iodide                 Fluorad FC-751 3M fluorinated amphoteric surfactant                            Fluorad FC-754 3M fluorinated alkyl quaternary ammonium chloride                               Fludrad FC-760 3M fluorinated alkanol EO                       Genapol UD-030 Hoechst C.sub.11 oxo alcohol 3EO                                Genapol UD-110 Hoechst C.sub.11 oxo alcohol 11EO                               Isopar V Exxon isoparaffinic oil                                               Kelzan Monsanto xanthan gum                                                    LI-700 Loveland lecithin-based adjuvant                                        Makon 4 Stepan nonylphenol 4EO                                                 Makon 6 Stepan nonylphenol 6EO                                                 Makon 30 Stepan nonylphenol 30EO                                               Makon NF-5 Stepan polyalkoxylated aliphatic base                               MON 0818 Monsanto tallowamine 15EO-based surfactant                            Myrj 52 ICI PEG-40 stearate                                                    Myrj 59 ICI PEG-100 stearate                                                   Nalco 1056 Nalco silica (26%)/aluminum oxide (4%); average particle                           size 20 nm                                                      Neodol 1-12 Shell C.sub.11 linear alcohol 12EO                                 Neodol 1-7 Shell C.sub.11 linear alcohol 7EO                                   Neodol 1-9 Shell C.sub.11 linear alcohol 9EO                                   Neodol 25-12 Shell C.sub.12-15 linear alcohol 12EO                             Neodol 25-20 Shell C.sub.12-15 linear alcohol 20EO                             Neodol 25-3 Shell C.sub.12-15 linear alcohol 3EO                               Neodol 25-7 Shell C.sub.12-15 linear alcohol 7EO                               Neodol 25-9 Shell C.sub.12-15 linear alcohol 9EO                               Neodol 45-13 Shell C.sub.14-15 linear alcohol 13EO                             Neodol 91-2.5 Shell C.sub.9-11 linear alcohol 2.5EO                            Neodox 25-11 Shell C.sub.12-15 linear alcohol ethoxycarboxylate 11EO                           Ninate 411 Stepan amine dodecylbenezene sulfonate                              Ninol 40-CO Stepan coco diethanolamide                         Orchex 796 Exxon paraffinic oil                                                Pluronic 31-R1 BASF 21PO-7EO-21PO block copolymer                              Pluronic F-108 BASF 128EO-54PO-128EO block copolymer                           Pluronic F-127 BASF 98EO-67PO-98EO block copolymer                             Pluronic F-68 BASF 75EO-30PO-75EO block copolymer                              Pluronic L-35 BASF 11EO-16PO-11EO block copolymer                              Pluronic L-43 BASF 7EO-21PO-7EO block copolymer                                Pluronic L-81 BASF 6EO-39PO-6EO block copolymer                                Pluronic P-84 BASF 27EO-39PO-27EO block copolymer                              Polystep B-25 Stepan decyl sulfate, Na salt                                    Reax 88B Westvaco highly sulfonated lignin, Na salt                            Sident 9 Degussa abrasive silica, 50 m.sup.2 /g                                Silwet 800 Witco heptamethyltrisiloxane EO                                     Silwet L-77 Witco heptamethyltrisiloxane 7EO methyl ether                      Simulsol SL-4 Seppic alkyl polyglucoside                                       Simulsol SL-10 Seppic alkyl polyglucoside                                      Simulsol SL-62 Seppic alkyl polyglucoside                                      Sipernat 22 Degussa hydrophilic precipitated silica, 190 m.sup.2 /g,                          av. aggregate size 100 μm                                    Sipernat 22S Degussa hydrophilic precipitated silica, 190 m.sup.2 /g,                         av. aggregate size <10 μm                                    Span 60 ICI sorbitan monostearate                                              Span 65 ICI sorbitan tristearate                                               Span 80 ICI sorbitan monooleate                                                Span 85 ICI sorbitan trioleate                                                 Steol CS-370 Stepan lauryl EO sulfate, Na salt                                 Stepanol WAC Stepan lauryl sulfate, Na salt                                    Stepfac 8170 Stepan nonylphenol EO phosphate                                   Surfynol 104 Air Products tetramethyldecyne diol                               Surfynol 465 Air Products tetramethyldecyne diol 10EO                          Tergitol 15-S-15 Union Carbide C.sub.15 branched secondary alcohol 15EO        Tergitol 15-S-20 Union Carbide C.sub.15 branched secondary alcohol 20EO        Tergitol 15-S-30 Union Carbide C.sub.15 branched secondary alcohol 30EO        Tergitol 15-S-40 Union Carbide C.sub.15 branched secondary alcohol 40EO        Titanium dioxide P25 Degussa titanium dioxide, average particle size 21                       nm                                                              Toximul 8240 Stepan PEG-36 castor oil                                          Toximul 8302 Stepan alcohol EO blend                                           Triton RW-20 Union Carbide alkylamine 2EO                                      Triton RW-50 Union Carbide alkylamine 5EO                                      Triton RW-75 Union Carbide alkylamine 7.5EO                                    Triton RW-100 Union Carbide alkylamine 10EO                                    Triton RW-150 Union Carbide alkylamine 15EO                                    Tryfac 5552 Henkel decyl EO phosphate, free acid                               Tween 20 ICI sorbitan monolaurate 20EO                                         Tween 40 ICI sorbitan monopalmitate 20EO                                       Tween 80 ICI sorbitan monooleate 20EO                                          Tween 85 ICI sorbitan trioleate 20EO                                           Velvetex AB-45 Henkel cocobetaine                                              Westvaco H-240 Westvaco dicarboxylate surfactant, K salt                     __________________________________________________________________________

Fluorad FC-135, though defined only generically as above in 3M product literature and in standard directories, has been specifically identified as

    C.sub.8 F.sub.17 SO.sub.2 NH(CH.sub.2).sub.3 N.sup.+ (CH.sub.3).sub.3 I.sup.-

in a paper by J. Linert & J. N. Chasman of 3M, titled "The effects of fluorochemical surfactants on recoatability" in the Dec. 20, 1993 issue of American Paint & Coatings Journal, and reprinted as a trade brochure by 3M. Fluorad FC-750 is believed to be based on the same surfactant. Fluorad FC-754 is believed to have the structure

    C.sub.8 F.sub.17 SO.sub.2 NH(CH.sub.2).sub.3 N.sup.+ (CH.sub.3).sub.3 Cl.sup.-

that is, identical to Fluorad FC-135 but with a chloride anion replacing iodide.

The following surfactants, identified in the Examples as "Surf H1" to "Surf H5", have hydrocarbyl groups as the hydrophobic moiety but otherwise bear some structural similarity to the above Fluorad surfactants. They were synthesized and characterized under contract to Monsanto Company.

Surf H1: C₁₂ H₂₅ SO₂ NH(CH₂)₃ N⁺ (CH₃)₃ I⁻

Surf H2: C₁₇ H₃₅ CONH(CH₂)₃ N⁺ (CH₃)₃ I⁻

Surf H3: C₁₁ H₂₃ CONH(CH₂)₃ N⁺ (CH₃)₃ I⁻

Surf H4: cis-C₈ H₁₇ CH═CH(CH₂)₇ CONH(CH₂)₃ N⁺ (CH₃)₃ I⁻

Surf H5: C₇ H₁₅ CONH(CH₂)₃ N⁺ (CH₃)₃ I⁻

Fatty alcohol ethoxylate surfactants are referred to in the Examples by their generic names as given in the International Cosmetic Ingredient Dictionary, 6th Edition, 1995 (Cosmetic, Toiletry and Fragrance Association, Washington, D.C.). They were interchangeably sourced from various manufacturers, for example:

Laureth-23: Brij 35 (ICI), Trycol 5964 (Henkel).

Ceteth-10: Brij 56 (ICI).

Ceteth-20: Brij 58 (ICI).

Steareth-10: Brij 76 (ICI).

Steareth-20: Brij 78 (ICI), Emthox 5888-A (Henkel), STA-20 (Heterene).

Steareth-30: STA-30 (Heterene).

Steareth-100: Brij 700 (ICI).

Ceteareth-15: CS-15 (Heterene).

Ceteareth-20: CS-20 (Heterene).

Ceteareth-27: Plurafac A-38 (BASF).

Ceteareth-55: Plurafac A-39 (BASF).

Oleth-2: Brij 92 (ICI).

Oleth-10: Brij 97 (ICI).

Oleth-20: Brij 98 (ICI), Trycol 5971 (Henkel).

Where a proprietary excipient is a surfactant supplied as a solution in water or other solvent, the amount to be used was calculated on a true surfactant basis, not an "as is" basis. For example, Fluorad FC-135 is supplied as 50% true surfactant, together with 33% isopropanol and 17% water; thus to provide a composition containing 0.1% w/w Fluorad FC-135 as reported herein, 0.2 g of the product as supplied was included in 100 g of the composition.

Spray compositions of the Examples contained an exogenous chemical, such as glyphosate IPA salt, in addition to the excipient ingredients listed. The amount of exogenous chemical was selected to provide the desired rate in grams per hectare (g/ha) when applied in a spray volume of 93 l/ha. Several exogenous chemical rates were applied for each composition. Thus, except where otherwise indicated, when spray compositions were tested, the concentration of exogenous chemical varied in direct proportion to exogenous chemical rate, but the concentration of excipient ingredients was held constant across different exogenous chemical rates.

Concentrate compositions were tested by dilution, dissolution or dispersion in water to form spray compositions. In these spray compositions prepared from concentrates, the concentration of excipient ingredients varied with that of exogenous chemical.

Except where otherwise indicated, these aqueous spray compositions were prepared by one of the following processes (i), (ii) or (iii).

(i) For compositions not containing lecithin or phospholipids, aqueous compositions were prepared by simple mixing of ingredients under mild agitation.

(ii) A weighed quantity of lecithin in powder form was dissolved in 0.4 ml chloroform in a 100 ml bottle. The resulting solution was air-dried to leave a thin film of lecithin, to which was added 30 ml deionized water. The bottle and its contents were then sonicated in a Fisher Sonic Dismembrator, Model 550, fitted with a 2.4 cm probe tip, set at output level 8, and operated continuously for 3 minutes. The resulting aqueous dispersion of lecithin was then allowed to cool to room temperature, and formed a lecithin stock which was later mixed in the required amounts with other ingredients under mild agitation. In some cases, as indicated in the Examples, certain ingredients were added to the lecithin in water before sonication, so that the lecithin and these ingredients were sonicated together. Without being bound by theory, it is believed that by sonicating a formulation ingredient together with lecithin, at least some of that ingredient becomes encapsulated within, or otherwise bound to or trapped by, vesicles or other aggregates formed by phospholipids present in the lecithin.

(iii) The procedure of process (ii) was followed except that, before sonication, the step of forming a lecithin solution in chloroform was omitted. Instead, lecithin in powder form was placed in a beaker, water was added and the beaker and its contents were then sonicated.

Except where otherwise indicated, aqueous concentrate compositions were prepared by one of the following processes (iv) to (x).

(iv) A weighed amount of lecithin powder of the type indicated was placed in a beaker and deionized water was added in no more than the amount required for the desired final composition. The beaker and its contents were then placed in a Fisher Sonic Dismembrator, Model 550, fitted with a 2.4 cm probe tip, set at output level 8, and operated for 5 minutes. The resulting lecithin dispersion formed the basis to which other ingredients were added with mild agitation to make the aqueous concentrate formulation. The order of addition of these ingredients was varied and was sometimes found to affect the physical stability of the concentrate formulation. Where a fluoro-organic surfactant such as Fluorad FC-135 or FC-754 was to be included, it was generally added first, followed by other surfactants if required and then by the exogenous chemical. Where the exogenous chemical used was glyphosate IPA salt, this was added in the form of a 62% (45% a.e.) solution by weight, at a pH of 4.4 to 4.6. A final adjustment with water took place if necessary as the last step. In some cases certain ingredients of the concentrate formulation were added before rather than after sonication, so that they were sonicated with the lecithin.

(v) A weighed amount of lecithin powder of the type indicated was placed in a beaker and deionized water was added in sufficient quantity to provide, after sonication as detailed below, a lecithin stock at a convenient concentration, normally in the range from 10% to 20% w/w and typically 15% w/w. The beaker and its contents were then placed in a Fisher Sonic Dismembrator, Model 550, fitted with a 2.4 cm probe tip with the pulse period set at 15 seconds with 1 minute intervals between pulses to allow cooling. Power output was set at level 8. After a total of 3 minutes of sonication (12 pulse periods) the resulting lecithin stock was finally adjusted to the desired concentration if necessary with deionized water. To prepare an aqueous concentrate formulation, the following ingredients were mixed in the appropriate proportions with mild agitation, normally in the order given although this was sometimes varied and was found in some cases to affect the physical stability of the concentrate formulation: (a) exogenous chemical, for example glyphosate IPA salt as a 62% w/w solution at pH 4.4-4.6; (b) lecithin stock; (c) other ingredients if required; and (d) water.

(vi) Water-in-oil-in-water (W/O/W) multiple emulsions were prepared as follows. First a water-in-oil emulsion was prepared. To do this, the required amounts of the selected oil and a first emulsifier (referred to in the Examples as "emulsifier #1") were mixed thoroughly. If it was desired to prepare the formulation with glyphosate in the inner aqueous phase, a measured amount of concentrated (62% w/w) aqueous solution of glyphosate IPA salt was added to the mixture of oil and first emulsifier with agitation to ensure homogeneity. The amount of water required in the inner aqueous phase was then added to complete the water-in-oil emulsion, which was finally subjected to high-shear mixing, typically using a Silverson L4RT-A mixer fitted with a fine emulsor screen operated for 3 minutes at 10,000 rpm. The required amount of a second emulsifier (referred to in the Examples as "emulsifier #2") was next added to the water-in-oil emulsion with agitation to ensure homogeneity. If it was desired to prepare the formulation with glyphosate in the outer aqueous phase, a measured amount of concentrated (62% w/w) aqueous solution of glyphosate IPA salt was added to the blend of the water-in-oil emulsion and the second emulsifier with further agitation. To complete the water-in-oil-in-water multiple emulsion composition, the amount of water required in the outer aqueous phase was added. The composition was finally subjected to high-shear mixing, typically using a Silverson L4RF-A mixer fitted with a medium emulsor screen, operated for 3 minutes at 7,000 rpm.

(vii) Oil-in-water (O/W) emulsions were prepared as follows. The required amount of the selected oil and surfactant (sometimes referred to in the Examples as "emulsifier #2" as it corresponds to the second emulsifier in process (vi)) were mixed thoroughly. If the surfactant selected was not free-flowing at ambient temperature, heat was applied to bring the surfactant into a flowable condition before mixing with the oil. A measured amount of concentrated (62% w/w) aqueous solution of glyphosate IPA salt was added to the surfactant-oil mixture with agitation. The required amount of water was added to bring the concentration of glyphosate and other ingredients to the desired level . The composition was finally subjected to high-shear mixing, typically using a Silverson L4RT-A mixer fitted with a medium emulsor screen, operated for 3 minutes at 7,000 rpm.

(viii) Surfactant-containing aqueous solution concentrates having no oil component were prepared as follows. A concentrated (62% w/w) aqueous solution of glyphosate IPA salt was added in the desired amount to a weighed quantity of the selected surfactant(s). If the surfactant selected is not free-flowing at ambient temperature, heat was applied to bring the surfactant into a flowable condition before adding the glyphosate solution. The required amount of water was added to bring the concentration of glyphosate and other ingredients to the desired level. The composition was finally subjected to high-shear mixing, typically using a Silverson L4RT-A mixer fitted with a medium emulsor screen, operated for 3 minutes at 7,000 rpm.

(ix) For compositions containing a colloidal particulate, the required amount by weight of the selected colloidal particulate was suspended in a concentrated (62% w/w) aqueous solution of glyphosate IPA salt and agitated with cooling to ensure homogeneity. To the resulting suspension was added the required amount by weight of the selected surfactant(s). For a surfactant which is not free-flowing at ambient temperature, heat was applied to bring the surfactant into a flowable condition before adding it to the suspension. In those instances where an oil, such as butyl stearate, was also to be included in the composition, the oil was first thoroughly mixed with the surfactant and the surfactant-oil mixture added to the suspension. To complete the aqueous concentrate, the required amount of water was added to bring the concentration of glyphosate and other ingredients to the desired level. The concentrate was finally subjected to high-shear mixing, typically using a Silverson L4RT-A mixer fitted with a medium emulsor screen, operated for 3 minutes at 7,000 rpm.

(x) The procedure for preparing aqueous concentrate formulations containing lecithin and butyl stearate was different from that followed for other lecithin-containing concentrates. Exogenous chemical, for example glyphosate IPA salt, was first added, with mild agitation, to deionized water in a formulation jar. The selected surfactant (other than lecithin) was then added, while continuing the agitation, to form a preliminary exogenous chemical/surfactant mixture. Where the surfactant is not free-flowing at ambient temperature, the order of addition was not as above. Instead, the non-free-flowing surfactant was first added to water together with any other surfactant (other than lecithin) required in the composition, and was then heated to 55° C. in a shaker bath for 2 hours. The resulting mixture was allowed to cool, then exogenous chemical was added with mild agitation to form the preliminary exogenous chemical/surfactant mixture. A weighed amount of the selected lecithin was added to the preliminary exogenous chemical/surfactant mixture, with stirring to break up lumps. The mixture was left for about 1 hour to allow the lecithin to hydrate, then butyl stearate was added, with further stirring until no phase separation occurred. The mixture was then transferred to a microfluidizer (Microfluidics International Corporation, Model M-110F) and microfluidized for 3 to 5 cycles at 10,000 psi (69 MPa). In each cycle, the formulation jar was rinsed with microfluidized mixture. In the last cycle, the finished composition was collected in a clean dry beaker.

The following procedure was used for testing compositions of the Examples to determine herbicidal effectiveness, except where otherwise indicated.

Seeds of the plant species indicated were planted in 85 mm square pots in a soil mix which was previously steam sterilized and prefertilized with a 14-14-14 NPK slow release fertilizer at a rate of 3.6 kg/m3. The pots were placed in a greenhouse with sub-irrigation. About one week after emergence, seedlings were thinned as needed, including removal of any unhealthy or abnormal plants, to create a uniform series of test pots.

The plants were maintained for the duration of the test in the greenhouse where they received a minimum of 14 hours of light per day. If natural light was insufficient to achieve the daily requirement, artificial light with an intensity of approximately 475 microcinsteins was used to make up the difference. Exposure temperatures were not precisely controlled but averaged about 27° C. during the day and about 18° C. during the night. Plants were sub-irrigated throughout the test to ensure adequate soil moisture levels.

Pots were assigned to different treatments in a fully randomized experimental design with 3 replications. A set of pots was left untreated as a reference against which effects of the treatments could later be evaluated.

Application of glyphosate compositions was made by spraying with a track sprayer fitted with a 9501E nozzle calibrated to deliver a spray volume of 93 liters per hectare (l/ha) at a pressure of 166 kilopascals (kPa). After treatment, pots were returned to the greenhouse until ready for evaluation.

Treatments were made using dilute aqueous compositions. These could be prepared as spray compositions directly from their ingredients, or by dilution with water of preformulated concentrate compositions.

For evaluation of herbicidal effectiveness, all plants in the test were examined by a single practiced technician, who recorded percent inhibition, a visual measurement of the effectiveness of each treatment by comparison with untreated plants. Inhibition of 0% indicates no effect, and inhibition of 100% indicates that all of the plants are completely dead. Inhibition of 85% or more is in most cases considered acceptable for normal herbicidal use; however in greenhouse tests such as those of the Examples it is normal to apply compositions at rates which give less than 85% inhibition, as this makes it easier to discriminate among compositions having different levels of effectiveness.

Example 1

Glyphosate-containing spray compositions were prepared by tank-mixing Formulations B and C with excipients as shown in Table 1.

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and 16 days after planting ECHCF, and evaluation of herbicidal inhibition was done 18 days after application. Results, averaged for all replicates of each treatment, are shown in Table 1.

                                      TABLE 1                                      __________________________________________________________________________     Glyphosate                                                                            Glyphosate rate Additive rate                                                                        % Inhibition                                      composition                                                                           g a.e./ha                                                                             Additive % v/v ABUTH                                                                               ECHCF                                        __________________________________________________________________________     Formulation C                                                                         175    none           40   75                                              350   69 89                                                                    500   97 100                                                                  Formulation B 175 none  45 37                                                   350   73 66                                                                    500   83 97                                                                   Formulation B 175 L-77 0.25 64 30                                               175  0.50 77 27                                                               Formulation B 175 FC-135 0.25 55 72                                             175  0.50 73 61                                                               Formulation B 175 FC-135 + L-77 8:1 0.50 71 58                                  175 FC-135 + L-77 4:1 0.50 76 61                                               175 FC-135 + L-77 2:1 0.50 63 56                                               175 FC-135 + L-77 1:1 0.50 77 40                                               175 FC-135 + L-77 1:2 0.50 54 23                                               175 FC-135 + L-77 1:4 0.50 76 31                                               175 FC-135 + L-77 1:8 0.50 53 29                                              Formulation B 175 FC-135 + L-77 8:1 0.25 51 48                                  175 FC-135 + L-77 4:1 0.25 37 47                                               175 FC-135 + L-77 2:1 0.25 45 37                                               175 FC-135 + L-77 1:1 0.25 65 27                                               175 FC-135 + L-77 1:2 0.25 45 29                                               175 FC-135 + L-77 1:4 0.25 60 17                                               175 FC-135 + L-77 1:8 0.25 52 15                                            __________________________________________________________________________

Tank mixtures of Fluorad FC-135 with Formulation B gave markedly superior herbicidal effectiveness on ABUTH by comparison with Formulation C, but did not match the herbicidal effectiveness of Formulation C on ECHCF. The antagonism of glyphosate activity on ECHCF seen with the nonionic organosilicone surfactant Silwet L-77 did not occur with the cationic fluoro-organic surfactant Fluorad FC-135.

Example 2

Aqueous spray compositions were prepared containing glyphosate sodium or IPA salts and excipient ingredients as shown in Table 2a. Process (ii) was followed for all compositions, using soybean lecithin (10-20% phospholipid, Sigma Type II-S). Without adjustment, the pH of the compositions was approximately 5. For those compositions having a pH of approximately 7 as shown in Table 2a, the pH was adjusted using the same base (sodium hydroxide or IPA) that formed the glyphosate salt.

                  TABLE 2a                                                         ______________________________________                                                   % w/w    Components                                                  Spray   Lecithin                                                                               Fluorad      sonicated                                                                              Glyphosate                                  composition g/l FC-135 L-77 with lecithin salt pH                            ______________________________________                                         2-01    5.0                  none    IPA     5                                   2-02 5.0  0.50 none IPA 5                                                      2-03 5.0   none Na 7                                                           2-04 5.0  0.50 none Na 7                                                       2-05 5.0   none IPA 7                                                          2-06 5.0  0.50 none IPA 7                                                      2-07 5.0   none Na 5                                                           2-08 5.0  0.50 none Na 5                                                       2-09 2.5   none IPA 5                                                          2-10 2.5 0.50  none IPA 5                                                      2-11 5.0 0.50  none IPA 5                                                      2-12 5.0 0.33 0.17 none IPA 5                                                  2-13 5.0  0.50 L-77 IPA 5                                                      2-14 5.0  0.50 L-77 Na 7                                                       2-15 5.0  0.50 L-77 IPA 7                                                      2-16 5.0  0.50 L-77 Na 5                                                     ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 17 days after application. Formulation C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 2b.

                  TABLE 2b                                                         ______________________________________                                         Spray       Glyphosate rate                                                                              % Inhibition                                         composition g a.e./ha     ABUTH    ECHCF                                       ______________________________________                                         Formulation C                                                                              100           8        54                                             200 54 75                                                                      300 77 90                                                                     Formulation C +  100 62 10                                                     Silwet L-77 0.5% v/v 200 91 25                                                  300 95 27                                                                     2-01 100 59 64                                                                  200 74 83                                                                      300 82 99                                                                     2-02 100 66 44                                                                  200 73 45                                                                      300 92 76                                                                     2-03 100 17 29                                                                  200 37 72                                                                      300 70 89                                                                     2-04 100 48 24                                                                  200 67 50                                                                      300 81 61                                                                     2-05 100 40 44                                                                  200 77 89                                                                      300 79 95                                                                     2-06 100 76 43                                                                  200 87 74                                                                      300 90 85                                                                     2-07 100 40 50                                                                  200 66 54                                                                      300 84 83                                                                     2-08 100 69 34                                                                  200 57 70                                                                      300 78 66                                                                     2-09 100 44 62                                                                  200 83 82                                                                      300 90 91                                                                     2-10 100 84 83                                                                  200 97 85                                                                      300 95 93                                                                     2-11 100 79 65                                                                  200 89 84                                                                      300 98 98                                                                     2-12 100 74 63                                                                  200 93 84                                                                      300 94 92                                                                     2-13 100 86 85                                                                  200 91 92                                                                      300 97 97                                                                     2-14 100 56 17                                                                  200 69 48                                                                      300 87 81                                                                     2-15 100 61 39                                                                  200 87 73                                                                      300 83 78                                                                     2-16 100 42 32                                                                  200 35 78                                                                      300 59 85                                                                   ______________________________________                                    

Surprisingly strong herbicidal effectiveness was observed with compositions 2-10 and 2-11 containing lecithin and Fluorad FC-135 on both ABUTH and ECHCF, by comparison with otherwise similar compositions (2-09 and 2-01) lacking the Fluorad FC-135. Herbicidal effectiveness of composition 2-11 at the 100 g a.e./ha glyphosate rate was superior to that of Formulation C at a threefold higher rate on ABUTH and superior to that of Formulation C at a twofold higher rate on ECHCF.

Example 3

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 3a. Process (ii), indicated in Table 3a as involving "high" sonication power, was followed for all compositions, except that for composition 3-06 a different sonication procedure, referred to as "low" sonication power, was used. In this procedure the lecithin in water was sonicated in a Fisher Model FS 14H ultrasonic bath for 30 minutes. Soybean lecithin (10-20% phospholipid, Sigma Type II-S) was used for all compositions. Without adjustment, the pH of the compositions was approximately 5. For those compositions having a pH of approximately 7 as shown in Table 3a, the pH was adjusted using the same base (sodium hydroxide or IPA) that formed the glyphosate salt.

                  TABLE 3a                                                         ______________________________________                                         Spray         % w/w                      Sonica-                               compo-                                                                               Lecithin                                                                               Fluorad      Components      tion                                  sition g/l FC-135 L-77 sonicated with lecithin pH power                      ______________________________________                                         3-01  5.0                  none        5   high                                  3-02 5.0  0.50 none 5 high                                                     3-03 5.0  0.50 L-77 5 high                                                     3-04 5.0  0.50 glyphosate 5 high                                               3-05 5.0  0.50 L-77, glyphosate 5 high                                         3-06 5.0   none 7 low                                                          3-07 5.0   none 7 high                                                         3-08 5.0  0.50 none 7 high                                                     3-09 5.0  0.50 L-77 7 high                                                     3-10 5.0  0.50 glyphosate 7 high                                               3-11 5.0  0.50 L-77, glyphosate 7 high                                         3-12 5.0 0.50  none 5 high                                                     3-13 5.0 0.50  FC-135 5 high                                                   3-14 5.0 0.50  glyphosate 5 high                                               3-15 5.0 0.17 0.33 FC-135, glyphosate 5 high                                   3-16 5.0 0.17 0.33 none 5 high                                                 3-17 5.0 0.17 0.33 FC-135, L-77 5 high                                         3-18 10.0   none 5 high                                                        3-19 20.0   none 5 high                                                        3-20 10.0  0.50 none 5 high                                                    3-21 10.0  0.50 L-77 5 high                                                    3-22 20.0  0.50 L-77 5 high                                                    3-23 20.0  0.50 L-77, glyphosate 5 high                                      ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 3b.

                  TABLE 3b                                                         ______________________________________                                         Spray       Glyphosate rate                                                                              % Inhibition                                         composition g a.e./ha     ABUTH    ECHCF                                       ______________________________________                                         Formulation B                                                                              100           11       12                                             200 55 43                                                                      300 65 38                                                                     Formulation B +  100 77 5                                                      Silwet L-77 0.5% v/v 200 95 10                                                  300 95 17                                                                     Formulation C 100 33 42                                                         200 63 98                                                                      300 85 99                                                                     Formulation C + 100 78 7                                                       Silwet L-77 0.5% v/v 200 95 19                                                  300 98 54                                                                     3-01 100 63 22                                                                  200 77 69                                                                      300 92 82                                                                     3-02 100 79 30                                                                  200 96 67                                                                      300 98 70                                                                     3-03 100 81 29                                                                  200 96 70                                                                      300 97 86                                                                     3-04 100 85 32                                                                  200 94 60                                                                      300 98 61                                                                     3-05 100 82 34                                                                  200 98 60                                                                      300 96 69                                                                     3-06 100 55 40                                                                  200 91 69                                                                      300 97 90                                                                     3-07 100 77 29                                                                  200 93 82                                                                      300 97 100                                                                    3-08 100 83 48                                                                  200 95 67                                                                      300 94 74                                                                     3-09 100 83 37                                                                  200 95 75                                                                      300 99 83                                                                     3-10 100 77 36                                                                  200 99 75                                                                      300 98 69                                                                     3-11 100 81 38                                                                  200 94 81                                                                      300 97 76                                                                     3-12 100 56 47                                                                  200 91 90                                                                      300 97 95                                                                     3-13 100 81 41                                                                  200 94 58                                                                      300 97 84                                                                     3-14 100 77 37                                                                  200 94 70                                                                      300 96 94                                                                     3-15 100 76 61                                                                  200 95 79                                                                      300 96 85                                                                     3-16 100 95 84                                                                  200 94 56                                                                      300 75 32                                                                     3-17 100 78 44                                                                  200 93 86                                                                      300 94 87                                                                     3-18 100 59 27                                                                  200 94 84                                                                      300 96 100                                                                    3-19 100 74 44                                                                  200 94 74                                                                      300 95 95                                                                     3-20 100 79 62                                                                  200 89 78                                                                      300 92 93                                                                     3-21 100 66 69                                                                  200 80 79                                                                      300 86 88                                                                     3-22 100 44 69                                                                  200 83 97                                                                      300 74 94                                                                     3-23 100 50 71                                                                  200 68 91                                                                      300 85 76                                                                   ______________________________________                                    

Composition 3-12 containing lecithin and Fluorad FC-135 again showed surprisingly high herbicidal effectiveness by comparison with composition 3-01, lacking the Fluorad FC-135, and also by comparison with Formulation C. When efforts were made to encapsulate Fluorad FC-135 or glyphosate (compositions 3-13 or 3-14 respectively) in lecithin liposomes by sonication in the presence of the ingredients sought to be encapsulated, some further enhancement of herbicidal effectiveness was evident on ABUTH, but effectiveness was reduced on ECHCF. Overall, the best activity in this test was obtained without encapsulation.

Example 4

Compositions 3-01 to 3-12 of Example 3 were tested in this Example. Black nightshade (Solanum nigrum, SOLNI) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 26 days after planting SOLNI and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 4.

                  TABLE 4                                                          ______________________________________                                                         Glyphosate rate                                                                           % Inhibition                                          Spray composition g a.e./ha SOLNI                                            ______________________________________                                         Formulation B   100        28                                                     200 35                                                                         300 70                                                                        Formulation B + 100 85                                                         Silwet L-77 0.5% v/v 200 98                                                     300 97                                                                        Formulation C 100 30                                                            200 58                                                                         300 70                                                                        Formulation C + 100 78                                                         Silwet L-77 0.5% v/v 200 82                                                     300 94                                                                        3-01 100 47                                                                     200 77                                                                         300 93                                                                        3-02 100 33                                                                     200 50                                                                         300 78                                                                        3-03 100 36                                                                     200 79                                                                         300 90                                                                        3-04 100 33                                                                     200 72                                                                         300 84                                                                        3-05 100 38                                                                     200 68                                                                         300 82                                                                        3-06 100 84                                                                     200 92                                                                         300 96                                                                        3-07 100 58                                                                     200 75                                                                         300 85                                                                        3-08 100 50                                                                     200 83                                                                         300 91                                                                        3-09 100 50                                                                     200 72                                                                         300 83                                                                        3-10 100 53                                                                     200 75                                                                         300 78                                                                        3-11 100 75                                                                     200 96                                                                         300 100                                                                       3-12 100 62                                                                     200 93                                                                         300 99                                                                      ______________________________________                                    

Composition 3-12 containing lecithin and Fluorad FC-135, as in the test of Example 3, showed remarkably strong herbicidal effectiveness, this time on SOLNI.

Example 5

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 5a. Process (ii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 5a                                                         ______________________________________                                                   % w/w                                                                Spray   Lecithin                                                                               Fluorad Silwet     Components                                    composition g/l FC-135 L-77 KCl sonicated with lecithin                      ______________________________________                                         5-01    5.0                        glyphosate                                    5-02 5.0  0.50  L-77                                                           5-03 5.0  0.50  L-77                                                           5-04 5.0  1.00  L-77                                                           5-05 5.0  0.20  none                                                           5-06 5.0  1.00  none                                                           5-07 5.0  0.20  L-77, glyphosate                                               5-08 5.0  0.50  L-77, glyphosate                                               5-09 5.0  1.00  L-77, glyphosate                                               5-10 2.5  0.10  L-77                                                           5-11 2.5  0.25  L-77                                                           5-12 2.5  0.50  L-77                                                           5-13 2.5  0.10  none                                                           5-14 2.5  0.25  none                                                           5-15 2.5  0.10  L-77, glyphosate                                               5-16 2.5  0.25  L-77, glyphosate                                               5-17 2.5  0.50  L-77, glyphosate                                               5-18 5.0  0.50 0.02 L-77                                                       5-19 5.0  0.50 0.02 L-77, glyphosate                                           5-20 5.0 0.50   none                                                           5-21 5.0 0.50   glyphosate                                                     5-22 5.0 0.33 0.17  none                                                       5-23 5.0 0.33 0.17  glyphosate                                               ______________________________________                                    

Velvetleaf Abutilon theophrasti, ABUTH) and Japanese millet Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 16 days after planting ECHCF, and evaluation of herbicidal inhibition was done 17 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 5b.

                  TABLE 5b                                                         ______________________________________                                                   Glyphosate rate                                                                            % Inhibition                                             Spray composition                                                                          g a.e./ha     ABUTH    ECHCF                                       ______________________________________                                         Formulation B                                                                              200           47       83                                             300 64 84                                                                      400 71 90                                                                     Formulation B +  200 83 58                                                     Silwet L-77 0.5% v/v 300 94 76                                                  400 100 85                                                                    Formulation C 200 46 96                                                         300 68 90                                                                      400 75 93                                                                     Formulation C + 200 81 66                                                      Silwet L-77 0.5% v/v 300 93 68                                                  400 96 86                                                                     5-01 200 70 91                                                                  300 74 100                                                                     400 93 94                                                                     5-02 200 81 95                                                                  300 68 100                                                                     400 81 100                                                                    5-03 200 78 100                                                                 300 99 83                                                                      400 98 99                                                                     5-04 200 89 95                                                                  300 93 95                                                                      400 86 100                                                                    5-05 200 60 89                                                                  300 79 100                                                                     400 86 100                                                                    5-06 200 76 100                                                                 300 84 100                                                                     400 100 96                                                                    5-07 200 65 97                                                                  300 78 97                                                                      400 77 100                                                                    5-08 200 82 100                                                                 300 95 100                                                                     400 96 100                                                                    5-09 200 78 99                                                                  300 89 99                                                                      400 90 100                                                                    5-10 200 66 100                                                                 300 79 98                                                                      400 89 100                                                                    5-11 200 67 95                                                                  300 81 100                                                                     400 97 100                                                                    5-12 200 76 88                                                                  300 79 100                                                                     400 95 96                                                                     5-13 200 59 85                                                                  300 66 93                                                                      400 67 100                                                                    5-14 200 56 89                                                                  300 67 100                                                                     400 83 100                                                                    5-15 200 54 100                                                                 300 63 100                                                                     400 78 100                                                                    5-16 200 46 88                                                                  300 73 100                                                                     400 86 100                                                                    5-17 200 81 98                                                                  300 83 97                                                                      400 92 96                                                                     5-18 200 56 92                                                                  300 64 100                                                                     400 74 100                                                                    5-19 200 64 94                                                                  300 80 97                                                                      400 80 96                                                                     5-20 200 88 91                                                                  300 96 100                                                                     400 98 98                                                                     5-21 200 92 94                                                                  300 100 100                                                                    400 100 100                                                                   5-22 200 88 97                                                                  300 93 95                                                                      400 95 100                                                                    5-23 200 79 100                                                                 300 96 100                                                                     400 97 96                                                                   ______________________________________                                    

Glyphosate activity on ECHCF in this test was too high to make meaningful comparisons. However, on ABUTH, composition 5-20 containing lecithin and Fluorad FC-135 exhibited remarkably strong herbicidal effectiveness by comparison with composition 5-01 (no Fluorad FC-135) and Formulation C. As in previous testing, a slight further advantage on ABUTH was obtained by efforts to encapsulate the glyphosate in lecithin liposomes, as in composition 5-21. Compositions 5-22 and 5-23, containing both Fluorad FC-135 and Silwet L-77 in addition to lecithin, also showed remarkably good herbicidal effectiveness.

Example 6

Compositions 5-01 to 5-23 of Example 5 were tested in this Example. Momingglory (Ipomoea spp., IPOSS) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after IPOSS and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 6.

                  TABLE 6                                                          ______________________________________                                                         Glyphosate rate                                                                           % Inhibition                                          Spray composition g a.e./ha IPOSS                                            ______________________________________                                         Formulation B   200        40                                                     400 66                                                                        Formulation B + 200 68                                                         Silwet L-77 0.5% v/v 400 79                                                    Formulation C 200 62                                                            400 71                                                                        Formulation C + 200 70                                                         Silwet L-77 0.5% v/v 400 72                                                    5-01 200 64                                                                     400 77                                                                        5-02 200 68                                                                     400 75                                                                        5-03 200 68                                                                     400 72                                                                        5-04 200 69                                                                     400 72                                                                        5-05 200 64                                                                     400 78                                                                        5-06 200 80                                                                     400 89                                                                        5-07 200 69                                                                     400 74                                                                        5-08 200 60                                                                     400 72                                                                        5-09 200 79                                                                     400 84                                                                        5-10 200 69                                                                     400 78                                                                        5-11 200 52                                                                     400 72                                                                        5-12 200 69                                                                     400 88                                                                        5-13 200 72                                                                     400 74                                                                        5-14 200 68                                                                     400 69                                                                        5-15 200 68                                                                     400 70                                                                        5-16 200 55                                                                     400 69                                                                        5-17 200 52                                                                     400 67                                                                        5-18 200 65                                                                     400 67                                                                        5-19 200 54                                                                     400 70                                                                        5-20 200 74                                                                     400 100                                                                       5-21 200 72                                                                     400 91                                                                        5-22 200 81                                                                     400 84                                                                        5-23 200 79                                                                     400 90                                                                      ______________________________________                                    

Once again, surprisingly strong herbicidal effectiveness, this time on IPOSS, was exhibited by compositions 5-20 to 5-23, all of which contain lecithin and Fluorad FC-135.

Example 7

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 7a. Process (ii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 7a                                                         ______________________________________                                                           % w/w         Components                                     Spray    Lecithin Fluorad  Silwet sonicated with                                 composition g/l FC-135 L-77 lecithin                                         ______________________________________                                         7-01     5.0               0.50   L-77                                           7-02 5.0  0.25 L-77                                                            7-03 5.0  0.10 L-77                                                            7-04 5.0   none                                                                7-05 2.5  0.50 L-77                                                            7-06 2.5  0.25 L-77                                                            7-07 2.5  0.10 L-77                                                            7-08 1.0  0.50 L-77                                                            7-09 1.0  0.25 L-77                                                            7-10 2.5  0.10 L-77                                                            7-11 2.5 0.25 0.25 L-77                                                        7-12 2.5 0.17 0.33 L-77                                                        7-13 2.5 0.33 0.17 L-77                                                        7-14 2.5 0.50  none                                                            7-15 2.5 0.25  none                                                            7-16 2.5 0.10  none                                                            7-17 2.5  0.25 glyphosate                                                      7-18 2.5  0.10 glyphosate                                                      7-19 2.5  0.50 glyphosate                                                      7-20 5.0  0.50 L-77, glyphosate                                                7-21 2.5  0.25 L-77, glyphosate                                                7-22 1.0  0.25 L-77, glyphosate                                                7-23 1.0  0.10 L-77, glyphosate                                              ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF), and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 20 days after planting ABUTH and ECHCF. Planting date for SIDSP was not recorded. Evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 7b.

                  TABLE 7b                                                         ______________________________________                                         Spray        Glyphosate rate                                                                           % Inhibition                                           composition  g a.e./ha  ABUTH    ECHCF SIDSP                                   ______________________________________                                         Formulation B                                                                               150        33       39    29                                         250 44 43 66                                                                   350 83 45 60                                                                  Formulation B +  150 81  7 46                                                  Silwet L-77 0.5% v/v 250 88 21 64                                               350 96 32 66                                                                  Formulation C 150 61 59 58                                                      250 77 92 85                                                                   350 91 92 83                                                                  Formulation C + 150 76 10 65                                                   Silwet L-77 0.5% v/v 250 87 17 60                                               350 92 39 64                                                                  7-01 150 87 43 47                                                               250 88 41 60                                                                   350 96 53 66                                                                  7-02 150 66 51 61                                                               250 85 81 63                                                                   350 84 89 75                                                                  7-03 150 66 54 65                                                               250 70 63 60                                                                   350 94 96 87                                                                  7-04 150 73 58 61                                                               250 85 83 90                                                                   350 91 100  83                                                                7-05 150 76 44 49                                                               250 85 55 56                                                                   350 93 79 64                                                                  7-06 150 64 73 56                                                               250 71 78 61                                                                   350 81 79 77                                                                  7-07 150 53 41 59                                                               250 74 78 68                                                                   350 78 90 75                                                                  7-08 150 83 33 59                                                               250 82 39 75                                                                   350 95 59 69                                                                  7-09 150 78 32 46                                                               250 85 42 75                                                                   350 91 62 67                                                                  7-10 150 26 36 43                                                               250 69 73 75                                                                   350 76 81 73                                                                  7-11 150 83 79 72                                                               250 96 93 78                                                                   350 99 97 84                                                                  7-12 150 78 57 58                                                               250 89 78 66                                                                   350 94 93 75                                                                  7-13 150 83 84 54                                                               250 94 93 67                                                                   350 99 97 93                                                                  7-14 150 80 68 69                                                               250 85 88 79                                                                   350 97 94 99                                                                  7-15 150 75 80 62                                                               250 93 93 76                                                                   350 95 91 94                                                                  7-16 150 75 69 60                                                               250 88 91 77                                                                   350 89 92 75                                                                  7-17 150 77 69 67                                                               250 88 91 86                                                                   350 93 97 96                                                                  7-18 150 71 63 66                                                               250 74 85 82                                                                   350 89 85 83                                                                  7-19 150 74 62 77                                                               250 86 80 93                                                                   350 92 96 96                                                                  7-20 150 39 46 38                                                               250 80 49 69                                                                   350 91 64 69                                                                  7-21 150 65 50 34                                                               250 64 52 52                                                                   350 78 67 62                                                                  7-22 150 68 18 35                                                               250 79 42 43                                                                   350 87 49 58                                                                  7-23 150 24 46 38                                                               250 62 49 42                                                                   350 91 53 67                                                                ______________________________________                                    

Compositions 7-14 to 7-16, containing 0.25% lecithin together with Fluorad FC-135, provided excellent herbicidal effectiveness on all three species tested. Even at the lowest concentration of Fluorad FC-135 (0.1% in composition 7-16), effectiveness was substantially maintained on ABUTH and ECHCF, although some loss of effectiveness was evident on SIDSP. Compositions 7-11 to 7-13, containing lecithin, Fluorad FC-135 and Silwet L-77, also performed well in this test, not showing the antagonism on ECHCF characteristic of compositions containing Silwet L-77 but no Fluorad FC-135.

Example 8

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 8a. Process (ii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti).

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 8a. The pH of all compositions was adjusted to approximately 7.

                  TABLE 8a                                                         ______________________________________                                                           % w/w         Components                                     Spray    Lecithin Fluorad  Silwet sonicated with                                 composition g/l FC-135 L-77 lecithin                                         ______________________________________                                         8-01     5.0               0.50   L-77                                           8-02 5.0  0.25 L-77                                                            8-03 5.0  0.10 L-77                                                            8-04 5.0   none                                                                8-05 2.5  0.50 L-77                                                            8-06 2.5  0.25 L-77                                                            8-07 2.5  0.10 L-77                                                            8-08 1.0  0.50 L-77                                                            8-09 1.0  0.25 L-77                                                            8-10 2.5  0.10 L-77                                                            8-11 2.5 0.25 0.25 L-77                                                        8-12 2.5 0.17 0.33 L-77                                                        8-13 2.5 0.33 0.17 L-77                                                        8-14 2.5 0.50  none                                                            8-15 2.5 0.25  none                                                            8-16 2.5 0.10  none                                                            8-17 2.5  0.25 glyphosate                                                      8-18 2.5  0.10 glyphosate                                                      8-19 2.5  0.50 glyphosate                                                    ______________________________________                                    

Yellow nutsedge (Cyperus esculentus, CYPES) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 21 days after planting CYPES, and evaluation of herbicidal inhibition was done 27 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 8b.

                  TABLE 8b                                                         ______________________________________                                         Spray           Glyphosate rate                                                                           % Inhibition                                          composition g a.e./ha CYPES                                                  ______________________________________                                         Formulation B    500       92                                                     1000 95                                                                        5000 100                                                                      Formulation B +  500 100                                                       Silwet L-77 0.5% v/v 1000 87                                                    5000 100                                                                      Formulation C  500 87                                                           1000 96                                                                        5000 100                                                                      Formulation C +  500 98                                                        Silwet L-77 0.5% v/v 1000 94                                                    5000 100                                                                      8-01  500 91                                                                    1000 100                                                                       1500 97                                                                       8-02  500 83                                                                    1000 100                                                                       1500 100                                                                      8-03  500 90                                                                    1000 88                                                                        1500 71                                                                       8-04  500 88                                                                    1000 100                                                                       1500 100                                                                      8-05  500 84                                                                    1000 99                                                                        1500 95                                                                       8-06  500 90                                                                    1000 88                                                                        1500 99                                                                       8-07  500 78                                                                    1000 94                                                                        1500 97                                                                       8-08  500 93                                                                    1000 96                                                                        1500 100                                                                      8-09  500 87                                                                    1000 88                                                                        1500 100                                                                      8-10  500 86                                                                    1000 100                                                                       1500 100                                                                      8-11  500 95                                                                    1000 94                                                                        1500 100                                                                      8-12  500 92                                                                    1000 92                                                                        1500 100                                                                      8-13  500 87                                                                    1000 97                                                                        1500 100                                                                      8-14  500 82                                                                    1000 100                                                                       1500 100                                                                      8-15  500 85                                                                    1000 90                                                                        1500 95                                                                       8-16  500 87                                                                    1000 91                                                                        1500 100                                                                      8-17  500 83                                                                    1000 90                                                                        1500 95                                                                       8-18  500 93                                                                    1000 100                                                                       1500 95                                                                       8-19  500 86                                                                    1000 95                                                                        1500 100                                                                    ______________________________________                                    

The commercial standard Formulation C exhibited very high herbicidal effectiveness in this test and for this reason it is not possible to discern enhancements. There is a suggestion at the lowest glyphosate rate (500 g a.e./ha), effectiveness of compositions containing lecithin and Fluorad FC-135 (8-14 to 8-16) on CYPES surprisingly improved with decreasing Fluorad FC-135 concentration.

Example 9

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 9a. Process (ii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 9                                                          ______________________________________                                                           % w/w         Components                                     Spray    Lecithin Fluorad  Silwet sonicated with                                 composition g/l FC-135 L-77 lecithin                                         ______________________________________                                         9-01     5.0                      none                                           9-02 5.0  0.50 none                                                            9-03 5.0  0.50 L-77                                                            9-04 2.5   none                                                                9-05 2.5  0.50 none                                                            9-06 2.5  0.50 L-77                                                            9-07 1.0   none                                                                9-08 1.0  0.50 none                                                            9-09 1.0  0.50 L-77                                                            9-10 0.5   none                                                                9-11 0.5  0.50 none                                                            9-12 0.5  0.50 L-77                                                            9-13 1.0  0.25 none                                                            9-14 1.0  0.25 L-77                                                            9-15 1.0  0.10 none                                                            9-16 1.0  0.10 L-77                                                            9-17 1.0 0.50  none                                                            9-18 1.0 0.20  none                                                            9-19 1.0 0.10  none                                                            9-20 0.5 0.50  none                                                            9-21 0.5 0.20  none                                                          ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. There was no record of the dates of planting. Evaluation of herbicidal inhibition was done 16 days after application.

In addition to compositions 9-01 to 9-21, spray compositions were prepared by tank mixing Formulations B and C with 0.5% Fluorad FC-135. Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 9b.

                  TABLE 9b                                                         ______________________________________                                         Spray         Glyphosate rate                                                                            % Inhibition                                         composition   g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         64        77                                            250 81 80                                                                      350 88 97                                                                     Formulation B +  150 42 38                                                     Silwet L-77 0.5% v/v 250 56 49                                                  350 67 64                                                                     Formulation C 150 61 89                                                         250 75 91                                                                      350 92 99                                                                     Formulation C + 150 92 40                                                      Silwet L-77 0.5% v/v 250 95 40                                                  350 94 74                                                                     Formulation B + 150 87 34                                                      Fluorad FC-135 0.5% w/v 250 90 44                                               350 97 47                                                                     Formulation C + 150 79 85                                                      Fluorad FC-135 0.5% w/v 250 77 86                                               350 92 91                                                                     9-01 150 75 69                                                                  250 84 89                                                                      350 98 98                                                                     9-02 150 86 54                                                                  250 96 74                                                                      350 99 86                                                                     9-03 150 86 66                                                                  250 91 77                                                                      350 96 86                                                                     9-04 150 68 73                                                                  250 97 85                                                                      350 94 92                                                                     9-05 150 90 55                                                                  250 96 69                                                                      350 91 82                                                                     9-06 150 87 43                                                                  250 91 68                                                                      350 97 83                                                                     9-07 150 56 76                                                                  250 81 88                                                                      350 89 96                                                                     9-08 150 85 35                                                                  250 93 51                                                                      350 98 66                                                                     9-09 150 94 45                                                                  250 97 47                                                                      350 98 52                                                                     9-10 150 62 60                                                                  250 85 78                                                                      350 93 88                                                                     9-11 150 90 32                                                                  250 92 42                                                                      350 98 59                                                                     9-12 150 93 38                                                                  250 93 56                                                                      350 95 72                                                                     9-13 150 85 39                                                                  250 89 66                                                                      350 94 79                                                                     9-14 150 83 70                                                                  250 93 45                                                                      350 93 70                                                                     9-15 150 65 54                                                                  250 85 79                                                                      350 91 89                                                                     9-16 150 75 65                                                                  250 83 79                                                                      350 90 84                                                                     9-17 150 81 94                                                                  250 88 97                                                                      350 100  99                                                                   9-18 150 79 89                                                                  250 95 91                                                                      350 98 98                                                                     9-19 150 77 85                                                                  250 91 96                                                                      350 95 97                                                                     9-20 150 77 71                                                                  250 86 92                                                                      350 100  93                                                                   9-21 150 75 91                                                                  250 84 97                                                                      350 96 95                                                                   ______________________________________                                    

Compositions of this Example (9-17 to 9-21) containing very low concentrations of lecithin and Fluorad FC-135 exhibited remarkably high herbicidal effectiveness. Even a composition (9-19) with just 0.1% lecithin and 0.1% Fluorad FC-135 was much more effective on ABUTH than commercial standard Formulation C, and equally as effective on ECHCF as Formulation C. The apparently strong antagonism on ECHCF seen when Formulation B was tank mixed with 0.5% Fluorad FC-135 in this test is uncharacteristic and has not been seen in other tests (see, for example, Example 12 herein); indeed the data for this set of treatments is so out of line that it is believed they may be due to an error in application.

Example 10

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 10a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 10a                                                        ______________________________________                                         Spray         % w/w               Components                                   compo-                                                                               Lecithin                                                                               Fluorad Silwet                                                                               Methyl                                                                               Sodium                                                                               sonicated with                           sition g/l FC-135 L-77 caprate cholate lecithin                              ______________________________________                                         10-01 5.0                               none                                     10-02 5.0  0.50   none                                                         10-03 5.0  0.50   L-77                                                         10-04 2.5     none                                                             10-05 0.5     none                                                             10-06 2.5  0.50   none                                                         10-07 2.5  0.50   L-77                                                         10-08 0.5  0.50   none                                                         10-09 0.5  0.50   L-77                                                         10-10 2.5 0.25    none                                                         10-11 2.5 0.10    none                                                         10-12 2.5 0.05    none                                                         10-13 0.5 0.25    none                                                         10-14 0.5 0.10    none                                                         10-15 0.5 0.05    none                                                         10-16 2.5   0.10  Me caprate                                                   10-17 2.5    0.10 Na cholate                                                 ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

In addition to compositions 10-01 to 10-17, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 10b.

                  TABLE 10b                                                        ______________________________________                                         Spray         Glyphosate rate                                                                            % Inhibition                                         composition   g a.e./ha   ABUTH     BCHCF                                      ______________________________________                                         Formulation B 200         53        69                                            300 76 85                                                                      400 77 81                                                                     Formulation B +  200 100  28                                                   Silwet L-77 0.5% v/v 300 100  35                                                400 100  47                                                                   Formulation C 200 57 81                                                         300 73 90                                                                      400 98 94                                                                     Formulation C + 200 99 28                                                      Silwet L-77 0.5% v/v 300 98 53                                                  400 99 56                                                                     Formulation B + 200 76 85                                                      Fluorad FC-135 0.25% w/v 300 95 81                                              400 100  100                                                                  Formulation B + 200 77 70                                                      Fluorad FC-135 0.1% w/v 300 94 81                                               400 98 87                                                                     Formulation B + 200 65 73                                                      Fluorad FC-135 0.05% w/v 300 84 94                                              400 88 96                                                                     Formulation C + 200 83 78                                                      Fluorad FC-135 0.25% w/v 300 98 94                                              400 97 95                                                                     Formulation C + 200 65 66                                                      Fluorad FC-135 0.1% w/v 300 89 86                                               400 97 89                                                                     Formulation C + 200 70 78                                                      Fluorad FC-135 0.05% w/v 300 79 84                                              400 96 98                                                                     10-01 200 93 71                                                                 300 91 89                                                                      400 97 97                                                                     10-02 200 95 59                                                                 300 97 68                                                                      400 99 79                                                                     10-03 200 97 55                                                                 300 98 62                                                                      400 100  76                                                                   10-04 200 83 72                                                                 300 87 84                                                                      400 95 100                                                                    10-05 200 69 78                                                                 300 92 93                                                                      400 98 97                                                                     10-06 200 94 61                                                                 300 99 67                                                                      400 100  76                                                                   10-07 200 99 52                                                                 300 99 63                                                                      400 100  80                                                                   10-08 200 96 47                                                                 300 99 57                                                                      400 99 55                                                                     10-09 200 99 23                                                                 300 98 58                                                                      400 100  53                                                                   10-10 200 89 91                                                                 300 91 99                                                                      400 98 100                                                                    10-11 200 81 91                                                                 300 91 99                                                                      400 92 100                                                                    10-12 200 66 96                                                                 300 86 100                                                                     400 94 99                                                                     10-13 200 80 97                                                                 300 98 98                                                                      400 99 100                                                                    10-14 200 68 92                                                                 300 89 100                                                                     400 99 98                                                                     10-15 200 84 95                                                                 300 94 100                                                                     400 97 100                                                                    10-16 200 73 94                                                                 300 89 100                                                                     400 99 100                                                                    10-17 200 58 94                                                                 300 77 96                                                                      400 90 90                                                                   ______________________________________                                    

Tank mixture of Fluorad FC-135 at concentrations as low as 0.05% with Formulation B resulted in remarkably strong herbicidal efficacy in this test. The antagonism on ECHCF seen with the nonionic organosilicone surfactant Silwet L-77 did not occur with the cationic fluoro-organic surfactant Fluorad FC-135. Noteworthy was the outstanding herbicidal effectiveness provided by a composition (10-15) containing just 0.05% lecithin and 0.05% Fluorad FC-135. In this test addition of 0.1% methyl caprate to 0.25% lecithin, the methyl caprate being sonicated together with the lecithin, enhanced performance on ECHCF but not on ABUTH (compare compositions 10-16 and 10-04).

Example 11

Compositions 10-01 to 10-17 of Example 10, and tank mixtures of Formulations B and C with Fluorad FC-135, were tested in this Example. Prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 22 days after planting SIDSP, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 11.

                  TABLE 11                                                         ______________________________________                                                           Glyphosate rate                                                                           % Inhibition                                        Spray composition g a.e./ha SIDSP                                            ______________________________________                                         Formulation B     200        46                                                   300 75                                                                         400 80                                                                        Formulation B + 200 96                                                         Silwet L-77 0.5% v/v 300 89                                                     400 87                                                                        Formulation C 200 80                                                            300 98                                                                         400 98                                                                        Formulation C + 200 75                                                         Silwet L-77 0.5% v/v 300 91                                                     400 94                                                                        Formulation B + 200 82                                                         Fluorad FC-135 0.25% w/v 300 94                                                 400 98                                                                        Formulation B + 200 70                                                         Fluorad FC-135 0.1% w/v 300 93                                                  400 88                                                                        Formulation B + 200 79                                                         Fluorad FC-135 0.05% w/v 300 92                                                 400 99                                                                        Formulation C + 200 79                                                         Fluorad FC-135 0.25% w/v 300 97                                                 400 97                                                                        Formulation C + 200 90                                                         Fluorad FC-135 0.1% w/v 300 96                                                  400 97                                                                        Formulation C + 200 80                                                         Fluorad FC-135 0.05% w/v 300 96                                                 400 99                                                                        10-01 200 93                                                                    300 97                                                                         400 98                                                                        10-02 200 71                                                                    300 89                                                                         400 89                                                                        10-03 200 71                                                                    300 87                                                                         400 98                                                                        10-04 200 76                                                                    300 100                                                                        400 100                                                                       10-05 200 91                                                                    300 99                                                                         400 97                                                                        10-06 200 57                                                                    300 95                                                                         400 88                                                                        10-07 200 64                                                                    300 68                                                                         400 94                                                                        10-08 200 89                                                                    300 96                                                                         400 99                                                                        10-09 200 80                                                                    300 77                                                                         400 94                                                                        10-10 200 90                                                                    300 94                                                                         400 98                                                                        10-11 200 81                                                                    300 100                                                                        400 96                                                                        10-12 200 86                                                                    300 92                                                                         400 95                                                                        10-13 200 86                                                                    300 99                                                                         400 100                                                                       10-14 200 97                                                                    300 100                                                                        400 100                                                                       10-15 200 99                                                                    300 100                                                                        400 100                                                                       10-16 200 92                                                                    300 100                                                                        400 100                                                                       10-17 200 92                                                                    300 99                                                                         400 100                                                                     ______________________________________                                    

Herbicidal effectiveness of Formulation C was very high on SIDSP in this test and accordingly enhancements are difficult to discern. However, remarkably strong performance was again seen with composition 10-15, containing just 0.05% lecithin and 5 0.05% Fluorad FC-135.

Example 12

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 12a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                                      TABLE 12a                                    __________________________________________________________________________              % w/w                  Components                                     Spray                                                                               Lecithin                                                                           Fluorad                                                                             Silwet    (*) Other                                                                              sonicated with                                   comp. g/l FC-135 L-77 Other (*) ingredient Lecithin                          __________________________________________________________________________     12-01                                                                               5.0                        none                                             12-02 5.0  0.50   L-77                                                         12-03 2.5     none                                                             12-04 2.5 0.50    none                                                         12-05 2.5 0.20    none                                                         12-06 2.5 0.10    none                                                         12-07 5.0   0.50 Diacid 1550 Diacid                                            12-08 5.0   0.10 Diacid 1550 Diacid                                            12-09 2.5   0.25 Diacid 1550 Diacid                                            12-10 2.5 0.25  0.05 Diacid 1550 Diacid                                        12-11 5.0 0.10  0.50 Genapol UD-030 Genapol                                    12-12 5.0 0.05  0.20 Genapol UD-030 Genapol                                    12-13 5.0 0.25  0.50 Neodol 25-3 Neodol                                        12-14 5.0 0.10  0.20 Neodol 25-3 Neodol                                      __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and momingglory (Ipomoea spp., IPOSS) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH, 18 days after planting ECHCF and 9 days after planting IPOSS. Evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 12-01 to 12-14, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 12b.

                  TABLE 12b                                                        ______________________________________                                                     Glyphosate                                                           rate % Inhibition                                                            Spray composition                                                                            g a.e./ha ABUTH    ECHCF IPOSS                                   ______________________________________                                         Formulation B 200       24       53    33                                         300 47 37 37                                                                   400 64 46 64                                                                  Formulation B + 200 85 3 66                                                    Silwet L-77 0.5% v/v 300 97 19 77                                               400 98 18 82                                                                  Formulation C 200 39 69 38                                                      300 71 90 67                                                                   400 87 100 76                                                                 Formulation C + 200 90 8 72                                                    Silwet L-77 0.5% v/v 300 95 50 79                                               400 100 90 73                                                                 Formulation B + 200 75 71 65                                                   Fluorad FC-135 0.5% w/v 300 94 92 79                                            400 98 100 77                                                                 Formulation B + 200 75 67 67                                                   Fluorad FC-135 0.25% w/v 300 85 73 71                                           400 96 97 75                                                                  Formulation B + 200 61 53 48                                                   Fluorad FC-135 0.1% w/v 300 82 98 72                                            400 95 86 70                                                                  Formulation C + 200 81 61 69                                                   Fluorad FC-135 0.5% w/v 300 75 75 71                                            400 84 84 77                                                                  Formulation C + 200 35 58 67                                                   Fluorad FC-135 0.25% w/v 300 68 97 64                                           400 92 96 73                                                                  Formulation C + 200 40 84 51                                                   Fluorad FC-135 0.1% w/v 300 79 94 58                                            400 99 86 74                                                                  12-01 200 69 69 62                                                              300 82 82 73                                                                   400 88 84 77                                                                  12-02 200 81 75 67                                                              300 83 74 72                                                                   400 95 93 75                                                                  12-03 200 48 69 70                                                              300 82 93 71                                                                   400 94 100 72                                                                 12-04 200 68 78 64                                                              300 90 94 76                                                                   400 96 99 79                                                                  12-05 200 75 86 68                                                              300 86 95 72                                                                   400 96 89 80                                                                  12-06 200 80 95 57                                                              300 85 82 60                                                                   400 96 91 73                                                                  12-07 200 41 72 64                                                              300 76 82 68                                                                   400 80 98 77                                                                  12-08 200 40 71 70                                                              300 51 91 76                                                                   400 77 98 72                                                                  12-09 200 43 74 64                                                              300 58 95 76                                                                   400 73 100 77                                                                 12-10 200 43 85 65                                                              300 74 75 65                                                                   400 83 99 76                                                                  12-11 200 39 71 66                                                              300 61 88 71                                                                   400 89 99 73                                                                  12-12 200 54 57 59                                                              300 79 77 75                                                                   400 89 84 71                                                                  12-13 200 69 72 69                                                              300 59 66 69                                                                   400 86 81 76                                                                  12-14 200 54 62 65                                                              300 65 77 69                                                                   400 84 81 74                                                                ______________________________________                                    

Tank mixtures of Formulation B with Fluorad FC-135 gave greater herbicidal effectiveness than Formulation C alone, without the attendant antagonism on ECHCF so characteristic of Silwet L-77. Addition of Fluorad FC-135 to glyphosate compositions containing 0.25% lecithin enhanced herbicidal effectiveness on ABUTH and ECHCF, but not, in this test, on IPOSS (compare compositions 12-04 to 12-06 with composition 12-03).

Example 13

Compositions 12-01 to 12-14 of Example 12, and tank mixtures of Formulations B and C with Fluorad FC-135, were tested in this Example. Prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 23 days after planting SIDSP, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 13.

                  TABLE 13                                                         ______________________________________                                                           Glyphosate rate                                                                           % Inhibition                                        Spray composition g a.e./ha SIDSP                                            ______________________________________                                         Formulation B     200        37                                                   300 47                                                                         400 50                                                                        Formulation B + 200 93                                                         Silwet L-77 0.5% v/v 300 100                                                    400 99                                                                        Formulation C 200 47                                                            300 63                                                                         400 86                                                                        Formulation C + 200 88                                                         Silwet L-77 0.5% v/v 300 92                                                     400 99                                                                        Formulation B + 200 51                                                         Fluorad FC-135 0.5% w/v 300 79                                                  400 84                                                                        Formulation B + 200 49                                                         Fluorad FC-135 0.25% w/v 300 53                                                 400 85                                                                        Formulation B + 200 44                                                         Fluorad FC-135 0.1% w/v 300 58                                                  400 70                                                                        Formulation C + 200 74                                                         Fluorad FC-135 0.5% w/v 300 89                                                  400 97                                                                        Formulation C + 200 52                                                         Fluorad FC-135 0.25% w/v 300 70                                                 400 75                                                                        Formulation C + 200 45                                                         Fluorad FC-135 0.1% w/v 300 74                                                  400 87                                                                        12-01 200 62                                                                    300 76                                                                         400 89                                                                        12-02 200 59                                                                    300 54                                                                         400 73                                                                        12-03 200 56                                                                    300 89                                                                         400 80                                                                        12-04 200 72                                                                    300 89                                                                         400 96                                                                        12-05 200 66                                                                    300 87                                                                         400 84                                                                        12-06 200 60                                                                    300 74                                                                         400 86                                                                        12-07 200 57                                                                    300 78                                                                         400 89                                                                        12-08 200 59                                                                    300 67                                                                         400 70                                                                        12-09 200 57                                                                    300 65                                                                         400 74                                                                        12-10 200 53                                                                    300 77                                                                         400 77                                                                        12-11 200 58                                                                    300 71                                                                         400 87                                                                        12-12 200 54                                                                    300 70                                                                         400 82                                                                        12-13 200 65                                                                    300 75                                                                         400 82                                                                        12-14 200 61                                                                    300 77                                                                         400 81                                                                      ______________________________________                                    

On SIDSP in this test, tank mix addition of Fluorad FC-135 to Formulation B enhanced herbicidal effectiveness over that obtained with Formulation C alone, only at the 0.5% concentration of Fluorad FC-135. Likewise, when added to a glyphosate composition containing 0.25% lecithin, Fluorad FC-135 enhanced herbicidal effectiveness most significantly at the 0.5% concentration (composition 12-04).

Example 14

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 14a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The following compositions had a pH of approximately 5: 14-01, 14-03, 14-07, 14-08, 14-10 and 14-12 to 14-17. All others were adjusted to a pH of approximately 7.

                  TABLE 14a                                                        ______________________________________                                         Spray          % w/w                                                           compo- Lecithin                                                                               Fluorad Silwet                                                                               Diacid                                                                               Components                                    sition g/l FC-135 L-77 1550 sonicated with lecithin                          ______________________________________                                         14-01  5.0                         none                                          14-02 5.0    none                                                              14-03 2.5    none                                                              14-04 2.5    none                                                              14-05 5.0    glyphosate                                                        14-06 5.0  0.50  L-77                                                          14-07 5.0  0.50  L-77                                                          14-08 2.5  0.50  L-77                                                          14-09 2.5  0.50  L-77                                                          14-10 2.5  0.25  glyphosate                                                    14-11 2.5  0.25  glyphosate                                                    14-12 2.5 0.25   none                                                          14-13 2.5 0.25   glyphosate                                                    14-14 2.5 0.10   none                                                          14-15 2.5 0.10   glyphosate                                                    14-16 2.5  0.25 0.25 L-77, Diacid                                              14-17 2.5  0.10 0.05 L-77, Diacid                                            ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and 20 days after planting ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

In addition to compositions 14-01 to 14-17, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at two concentrations. Formulations B and C, alone and tank mixed with 0.5% and 0.25% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 14b.

                  TABLE 14b                                                        ______________________________________                                                     Glyphosate rate                                                                           % Inhibition                                            Spray composition                                                                            g a.e./ha    ABUTH    ECHCF                                      ______________________________________                                         Formulation B 200          53       43                                            300 73 50                                                                      400 91 74                                                                     Formulation B +  200 86 24                                                     Silwet L-77 0.5% v/v 300 88 15                                                  400 94 58                                                                     Formulation B + 200 80 22                                                      Silwet L-77 0.25% W/V 300 93 38                                                 400 87 38                                                                     Formulation C 200 56 88                                                         300 86 98                                                                      406 94 98                                                                     Formulation C + 200 87 23                                                      Silwet L-77 0.5% v/v 300 93 52                                                  400 91 60                                                                     Formulation C + 290 79 42                                                      Silwet L-77 0.25% v/v 300 83 73                                                 400 87 95                                                                     Formulation B + 200 79 49                                                      Fluorad FC-135 0.25% w/v 300 89 77                                              400 94 85                                                                     Formulation B + 200 73 64                                                      Fluorad FC-135 0.1% w/v 300 89 68                                               400 92 75                                                                     Formulation C + 200 73 86                                                      Fluorad FC-135 0.25% w/v 300 75 90                                              400 90 95                                                                     Formulation C + 200 53 97                                                      Fluorad FC-135 0.1% w/v 300 89 96                                               400 91 99                                                                     14-01 200 71 66                                                                 300 89 62                                                                      400 97 85                                                                     14-02 200 83 52                                                                 300 89 72                                                                      400 82 93                                                                     14-03 200 54 53                                                                 300 89 84                                                                      400 93 77                                                                     14-04 200 81 38                                                                 300 94 76                                                                      400 98 88                                                                     14-05 200 85 53                                                                 300 95 80                                                                      400 94 91                                                                     14-06 200 80 0                                                                  300 95 100                                                                     400 98 94                                                                     14-07 200 72 50                                                                 300 95 84                                                                      400 98 92                                                                     14-08 200 81 69                                                                 300 99 83                                                                      400 100 80                                                                    14-09 200 86 38                                                                 300 94 80                                                                      400 96 90                                                                     14-10 200 58 67                                                                 300 82 85                                                                      400 92 90                                                                     14-11 200 83 64                                                                 300 88 74                                                                      400 90 88                                                                     14-12 200 89 90                                                                 300 100 88                                                                     400 100 98                                                                    14-13 200 95 91                                                                 300 93 97                                                                      400 100 98                                                                    14-14 200 88 93                                                                 300 93 85                                                                      400 98 90                                                                     14-15 200 85 87                                                                 300 98 98                                                                      400 96 100                                                                    14-16 200 76 72                                                                 300 83 87                                                                      400 89 97                                                                     14-17 200 53 67                                                                 300 48 62                                                                      400 82 85                                                                   ______________________________________                                    

Compositions 14-12 to 14-15, containing 0.25% lecithin together with Fluorad FC-135, exhibited much greater herbicidal effectiveness on both ABUTH and ECHCF than composition 14-03, containing 0.25% lecithin but no Fluorad FC-135, or even composition 14-01, containing 0.5% lecithin but no Fluorad FC-135. No great or consistent difference was seen between compositions where glyphosate had been sonicated together with the lecithin (14-13 and 14-15) than where the lecithin had been sonicated alone (14-12 and 14-14).

Example 15

Compositions 14-01 to 14-17 of Example 14, and tank mixtures of Formulations B and C with Fluorad FC-135, were tested in this Example. Prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 22 days after planting SIDSP, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and C, alone and tank mixed with 0.5% Silwet L-77, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 15.

                  TABLE 15                                                         ______________________________________                                                        Glyphosate rate                                                                         % Inhibition                                           Spray composition                                                                               g a.e./ha  SIDSP                                              ______________________________________                                         Formulation B    200        23                                                    300 37                                                                         400 32                                                                        Formulation B + 200 30                                                         Silwet L-77 0.5% v/v 300 39                                                     400 45                                                                        Formulation B + 200 28                                                         Silwet L-77 0.25% w/v 300 49                                                    400 28                                                                        Formulation C 200 41                                                            300 54                                                                         400 84                                                                        Formulation C + 200 43                                                         Silwet L-77 0.5% v/v 300 66                                                     400 86                                                                        Formulation C + 200 17                                                         Silwet L-77 0.25% v/v 300 35                                                    400 58                                                                        Formulation B + 200 48                                                         Fluorad FC-135 0.25% w/v 300 60                                                 400 62                                                                        Formulation B + 200 31                                                         Fluorad FC-135 0.1% w/v 300 47                                                  400 75                                                                        Formulation C + 200 43                                                         Fluorad FC-135 0.25% w/v 300 57                                                 400 71                                                                        Formulation C + 200 32                                                         Fluorad FC-135 0.1% w/v 300 71                                                  400 63                                                                        14-01 200 51                                                                    300 55                                                                         400 76                                                                        14-02 200 51                                                                    300 68                                                                         400 84                                                                        14-03 200 55                                                                    300 51                                                                         400 72                                                                        14-04 200 50                                                                    300 64                                                                         400 75                                                                        14-05 200 46                                                                    300 53                                                                         400 61                                                                        14-06 200 40                                                                    300 44                                                                         400 73                                                                        14-07 200 23                                                                    300 32                                                                         400 39                                                                        14-08 200 18                                                                    300 44                                                                         400 57                                                                        14-09 200 25                                                                    300 30                                                                         400 43                                                                        14-10 200 19                                                                    300 36                                                                         400 38                                                                        14-11 200 35                                                                    300 48                                                                         400 57                                                                        14-12 200 65                                                                    300 80                                                                         400 88                                                                        14-13 200 68                                                                    300 75                                                                         400 87                                                                        14-14 200 76                                                                    300 76                                                                         400 72                                                                        14-15 200 54                                                                    300 73                                                                         400 84                                                                        14-16 200 44                                                                    300 51                                                                         400 63                                                                        14-17 200 23                                                                    300 45                                                                         400 57                                                                      ______________________________________                                    

Compositions 14-12 to 14-15, containing 0.25% lecithin together with Fluorad FC-135, exhibited greater herbicidal effectiveness on SIDSP than composition 14-03, containing 0.25% lecithin but no Fluorad FC-135, or even composition 14-01, containing 0.5% lecithin but no Fluorad FC-135. No great or consistent difference was seen between compositions where glyphosate had been sonicated together with the lecithin (14-13 and 14-15) than where the lecithin had been sonicated alone (14-12 and 14-14).

Example 16

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 16a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 16a                                                        ______________________________________                                                 % w/w                                                                  Spray Lecithin                                                                               Fluorad Other (*) Other                                                                             Components sonicated                          comp. g/l FC-135 (*) ingredient with lecithin                                ______________________________________                                         16-01 2.5                          none                                          16-02 2.5    glyphosate                                                        16-03 2.5 0.25   none                                                          16-04 2.5 0.25   glyphosate                                                    16-05 2.5  0.25 Silwet 800 none                                                16-06 2.5  0.25 Silwet 800 Silwet 800                                          16-07 2.5  0.25 Silwet 800 Silwet, glyphosate                                  16-08 0.5    none                                                              16-09 0.5    glyphosate                                                        16-10 0.5 0.05   none                                                          16-11 0.5 0.05   glyphosate                                                    16-12 0.5 0.03 0.02 Silwet Silwet L-77                                             L-77                                                                       16-13 0.5  0.05 methyl Me caprate                                                  caprate                                                                    16-14 0.5 0.05 0.05 methyl Me caprate                                              caprate                                                                    16-15 0.5 0.05 0.05 methyl Me caprate, glyphosate                                  caprate                                                                    16-16 0.5  0.01 PVA none                                                       16-17 0.5  0.01 PVA glyphosate                                                 16-18 0.5 0.05 0.01 PVA glyphosate                                             16-19 0.5  0.05 +  L-77 + Silwet L-77                                             0.01 PVA                                                                  ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 17 days after application.

In addition to compositions 16-01 to 16-19, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at two concentrations. Formulations B and C, alone and tank mixed with 0.5% Silwet 800, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 16b.

                  TABLE 16b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Spray composition                                                                            g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         13        28                                            250 37 51                                                                      350 56 38                                                                     Formulation B +  150 81 15                                                     Silwet 800 0.25% v/v 250 89 17                                                  350 91 20                                                                     Formulation C 150 32 65                                                         250 59 91                                                                      350 85 89                                                                     Formulation C + 150 91 17                                                      Silwet 800 0.25% v/v 250 91 23                                                  350 95 48                                                                     Formulation B + 150 31 58                                                      Fluorad FC-135 0.25% w/v 250 53 68                                              350 71 84                                                                     Formulation B + 150 31 29                                                      Fluorad FC-135 0.05% w/v 250 44 69                                              350 95 79                                                                     Formulation C + 150 46 45                                                      Fluorad FC-135 0.25% w/v 250 69 79                                              350 86 77                                                                     Formulation C + 150 44 57                                                      Fluorad FC-135 0.05% w/v 250 60 87                                              350 86 88                                                                     16-01 150 55 50                                                                 250 87 81                                                                      350 89 88                                                                     16-02 150 56 54                                                                 250 89 69                                                                      350 87 98                                                                     16-03 150 89 68                                                                 250 89 84                                                                      350 91 90                                                                     16-04 150 63 68                                                                 250 89 86                                                                      350 99 89                                                                     16-05 150 81 51                                                                 250 87 84                                                                      350 94 26                                                                     16-06 150 67  0                                                                 250 93 62                                                                      350 94 81                                                                     16-07 150 81 35                                                                 250 84 51                                                                      350 95 62                                                                     16-08 150 59 51                                                                 250 84 69                                                                      350 98 90                                                                     16-09 150 64 59                                                                 250 85 61                                                                      350 94 96                                                                     16-10 150 73 74                                                                 250 87 83                                                                      350 98 96                                                                     16-11 150 76 64                                                                 250 88 79                                                                      350 94 81                                                                     16-12 150 59 46                                                                 250 82 88                                                                      350 92 82                                                                     16-13 150 61 45                                                                 250 90 69                                                                      350 93 90                                                                     16-14 150 76 50                                                                 250 95 73                                                                      350 99 91                                                                     16-15 150 78 67                                                                 250 95 80                                                                      350 99 85                                                                     16-16 150 48 42                                                                 250 77 87                                                                      350 87 75                                                                     16-17 150 47 63                                                                 250 85 67                                                                      350 90 78                                                                     16-18 150 55 46                                                                 250 82 77                                                                      350 90 87                                                                     16-19 150 32 23                                                                 250 43 31                                                                      350 76 65                                                                   ______________________________________                                    

As in Example 10, glyphosate compositions (16-10 and 16-11) containing just 0.05% lecithin and 0.05% Fluorad FC-135 exhibited surprisingly great herbicidal efficacy in this test. Sonicating the lecithin in the presence of glyphosate in an effort to encapsulate some of the glyphosate (composition 16-11) did not give an advantage in performance over sonicating the lecithin alone (composition 16-10); indeed on ECHCF herbicidal efficacy was slightly better without such efforts to encapsulate the glyphosate. Addition of methyl caprate to compositions containing lecithin with or without Fluorad FC-135 (16-13 to 16-15) improved herbicidal effectiveness on ABUTH but had little effect on ECHCF.

Example 17

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 17a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 17a                                                        ______________________________________                                                   % w/w               Components                                       Spray   Lecithin                                                                               Fluorad Other                                                                               (*) Other                                                                               sonicated with                             composition g/l FC-135 (*) ingredient lecithin                               ______________________________________                                         17-01   2.5                           none                                       17-02 2.5 0.25   none                                                          17-03 2.5 0.25   glyphosate                                                    17-04 2.5 0.25 0.025 PVA none                                                  17-05 1.0    none                                                              17-06 1.0    glyphosate                                                        17-07 1.0 0.10   none                                                          17-08 1.0 0.10   glyphosate                                                    17-09 1.0 0.05   none                                                          17-10 1.0 0.05   glyphosate                                                    17-11 1.0  0.100 PVA none                                                      17-12 1.0  0.025 PVA none                                                      17-13 1.0 0.05 0.025 PVA none                                                  17-14 1.0  0.100 sodium cholate Na cholate                                     17-15 1.0  0.020 sodium cholate Na cholate                                     17-16 1.0 0.05 0.020 sodium cholate Na cholate                                 17-17 0.5    none                                                              17-18 0.5 0.05   glyphosate                                                    17-19 0.5 0.05 0.020 sodium cholate Na cholate                               ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

In addition to compositions 17-01 to 17-19, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 17b.

                  TABLE 17b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Spray composition                                                                            g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 200         32        25                                            300 50 34                                                                      400 54 35                                                                     Formulation C 200 59 92                                                         300 76 100                                                                     400 93 97                                                                     Formulation B + 200 43 48                                                      Fluorad FC-135 0.25% w/v 300 64 52                                              400 84 71                                                                     Formulation B + 200 61 78                                                      Fluorad FC-135 0.1% w/v 300 65 59                                               400 100  86                                                                   Formulation B + 200 58 30                                                      Fluorad FC-135 0.05% w/v 300 82 55                                              400 88 77                                                                     Formulation C + 200 53 55                                                      Fluorad FC-135 0.25% w/v 300 76 68                                              400 88 93                                                                     Formulation C + 200 59 70                                                      Fluorad FC-135 0.1% w/v 300 89 85                                               400 93 83                                                                     Formulation C + 200 60 72                                                      Fluorad FC-135 0.05% w/v 300 82 100                                             400 94 94                                                                     17-01 200 73 52                                                                 300 88 80                                                                      400 94 90                                                                     17-02 200 83 80                                                                 300 96 83                                                                      400 97 95                                                                     17-03 200 86 73                                                                 300 95 79                                                                      400 98 94                                                                     17-04 200 73 72                                                                 300 94 86                                                                      400 96 93                                                                     17-05 200 67 68                                                                 300 94 74                                                                      400 96 91                                                                     17-06 200 65 61                                                                 300 79 82                                                                      400 91 81                                                                     17-07 200 75 65                                                                 300 92 84                                                                      400 98 91                                                                     17-08 200 66 70                                                                 300 87 96                                                                      400 97 97                                                                     17-09 200 83 73                                                                 300 91 83                                                                      400 97 89                                                                     17-10 200 89 70                                                                 300 92 79                                                                      400 91 74                                                                     17-11 200 65 58                                                                 300 86 86                                                                      400 97 100                                                                    17-12 200 75 64                                                                 300 79 85                                                                      400 91 87                                                                     17-13 200 79 53                                                                 300 81 83                                                                      400 96 88                                                                     17-14 200 56 69                                                                 300 80 95                                                                      400 92 93                                                                     17-15 200 57 77                                                                 300 67 91                                                                      400 88 90                                                                     17-16 200 88 82                                                                 300 85 87                                                                      400 76 72                                                                     17-17 200 53 66                                                                 300 71 72                                                                      400 87 83                                                                     17-18 200 89 85                                                                 300 79 72                                                                      400 65 60                                                                     17-19 200 77 65                                                                 300 87 85                                                                      400 92 94                                                                   ______________________________________                                    

In glyphosate compositions containing lecithin and Fluorad FC-135, no consistent difference in herbicidal effectiveness was observed between those where lecithin was sonicated alone (17-02, 17-07, 17-09) and those where glyphosate and lecithin were sonicated together (17-03, 17-08, 17-10). The anomalous inversion of the apparent rate response to glyphosate seen with composition 17-18 is believed to be the result of an error in application or recording and the data for this composition should be ignored in this Example.

Example 18

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 18a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 18a                                                        ______________________________________                                                    % w/w                                                               Spray    Lecithin                                                                               Fluorad        Components                                       composition g/l FC-135 PVA sonicated with lecithin                           ______________________________________                                         18-01    2.5                    none                                             18-02 1.0   none                                                               18-03 0.5   none                                                               18-04 0.2   none                                                               18-05 1.0 0.25  none                                                           18-06 1.0 0.25  glyphosate                                                     18-07 1.0 0.10  none                                                           18-08 1.0 0.10  glyphosate                                                     18-09 0.5 0.05  none                                                           18-10 0.5 0.05  glyphosate                                                     18-11 2.5  0.10 none                                                         ______________________________________                                    

Hemp sesbania (Sesbania exaltata, SEBEX) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 22 days after planting SEBEX, and evaluation of herbicidal inhibition was done 21 days after application.

In addition to compositions 18-01 to 18-11, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone, and Formulation B tank mixed with 0.1% PVA (polyvinyl alcohol), were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 18b.

                  TABLE 18b                                                        ______________________________________                                                          Glyphosate rate                                                                           % Inhibition                                         Spray composition g a.e./ha SEBEX                                            ______________________________________                                         Formulation B     500       43                                                    1000 54                                                                        1500 44                                                                       Formulation B +  500 53                                                        PVA 0.1% w/v 1000 45                                                            1500 44                                                                       Formulation C  500 56                                                           1000 62                                                                        1500 63                                                                       Formulation B +  500 40                                                        Fluorad FC-135 0.25% w/v 1000 45                                                1500 60                                                                       Formulation B +  500 33                                                        Fluorad FC-135 0.1% w/v 1000 51                                                 1500 53                                                                       Formulation B +  500 21                                                        Fluorad FC-135 0.05% w/v 1000 18                                                1500 29                                                                       Formulation C +  500 34                                                        Fluorad FC-135 0.25% w/v 1000 41                                                1500 58                                                                       Formulation C +  500 50                                                        Fluorad FC-135 0.1% w/v 1000 43                                                 1500 52                                                                       Formulation C +  500 48                                                        Fluorad FC-135 0.05% w/v 1000 49                                                1500 46                                                                       18-01  500 22                                                                   1000 33                                                                        1500 37                                                                       18-02  500 16                                                                   1000 24                                                                        1500 28                                                                       18-03  500 15                                                                   1000 24                                                                        1500 27                                                                       18-04  500 17                                                                   1000 13                                                                        1500 31                                                                       18-05  500 28                                                                   1000 64                                                                        1500 68                                                                       18-06  500 64                                                                   1000 51                                                                        1500 61                                                                       18-07  500 65                                                                   1000 51                                                                        1500 63                                                                       18-08  500 50                                                                   1000 56                                                                        1500 30                                                                       18-09  500 40                                                                   1000 59                                                                        1500 66                                                                       18-10  500 31                                                                   1000 23                                                                        1500 49                                                                       18-11  500 43                                                                   1000 39                                                                        1500 74                                                                     ______________________________________                                    

Glyphosate activity on SEBEX was extremely weak in this test and no firm conclusions can be drawn.

Example 19

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 19a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 19a                                                        ______________________________________                                         Spray   Lecithin % w/w        Components                                         composition g/l Fluorad FC-135 sonicated with lecithin                       ______________________________________                                         19-01   2.5                   none                                               19-02 1.0  none                                                                19-03 0.5  none                                                                19-04 0.2  none                                                                19-05 1.0 0.25 none                                                            19-06 1.0 0.25 glyphosate                                                    ______________________________________                                    

Sicklepod (Cassia obtusifolia, CASOB) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 22 days after planting CASOB, and evaluation of herbicidal inhibition was done 21 days after application.

In addition to compositions 19-01 to 19-06, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at two concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 19b.

                  TABLE 19b                                                        ______________________________________                                                        Glyphosate rate                                                                         % Inhibition                                           Spray composition                                                                               g a.e./ha  CASOB                                              ______________________________________                                         Formulation B    500        35                                                    800 37                                                                         1200 34                                                                       Formulation C 500 49                                                            800 49                                                                         1200 66                                                                       Formulation B + 500 45                                                         Fluorad FC-135 0.25% w/v 800 50                                                 1200 71                                                                       Formulation B + 500 49                                                         Fluorad FC-135 0.1% w/v 800 49                                                  1200 78                                                                       Formulation C + 500 60                                                         Fluorad FC-135 0.25% w/v 800 75                                                 1200 68                                                                       Formulation C + 500 47                                                         Fluorad FC-135 0.1% w/v 800 85                                                  1200 74                                                                       19-01 500 54                                                                    800 51                                                                         1200 43                                                                       19-02 500 37                                                                    800 69                                                                         1200 52                                                                       19-03 500 35                                                                    800 51                                                                         1200 43                                                                       19-04 500 71                                                                    800 69                                                                         1200 57                                                                       19-05 500 47                                                                    800 73                                                                         1200 89                                                                       19-06 500 49                                                                    800 51                                                                         1200 73                                                                     ______________________________________                                    

On CASOB, the addition of Fluorad FC-135 to a glyphosate composition containing lecithin significantly enhanced herbicidal effectiveness (compare compositions 19-05 and 19-02). However, where glyphosate was sonicated together with the lecithin (composition 19-06), herbicidal effectiveness was reduced.

Example 20

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 20a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 20a                                                        ______________________________________                                                     % w/w                                                              Spray   Lecithin  Fluorad Diacid                                                                               Components                                       composition g/l FC-135 1550 sonicated with lecithin                          ______________________________________                                         20-01   2.5                     none                                             20-02 0.5   none                                                               20-03 0.2   none                                                               20-04 2.5 0.05  none                                                           20-05 0.5 0.05  none                                                           20-06 0.2 0.05  none                                                           20-07 0.5  0.05 Diacid                                                       ______________________________________                                    

Common lambsquarter (Chenopodium album, CHEAL) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 31 days after planting CHEAL, and evaluation of herbicidal inhibition was done 18 days after application.

In addition to compositions 20-01 to 20-07, spray compositions were prepared by tank mixing Formulations B and C with 0.5% Fluorad FC-135. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 20b.

                  TABLE 20b                                                        ______________________________________                                                        Glyphosate rate                                                                         % Inhibition                                           Spray composition                                                                               g a.e./ha  CHEAL                                              ______________________________________                                         Formulation B    150        0                                                     250 0                                                                          350 3                                                                         Formulation C 150 18                                                            250 68                                                                         350 98                                                                        Formulation B + 150 0                                                          Fluorad FC-135 0.05% w/v 250 10                                                 350 5                                                                         Formulation C + 150 3                                                          Fluorad FC-135 0.05% w/w 250 50                                                 350 60                                                                        20-01 150 0                                                                     250 27                                                                         350 60                                                                        20-02 150 0                                                                     250 5                                                                          350 8                                                                         20-03 150 5                                                                     250 0                                                                          350 8                                                                         20-04 150 18                                                                    250 29                                                                         350 63                                                                        20-05 150 17                                                                    250 14                                                                         350 87                                                                        20-06 150 44                                                                    250 40                                                                         350 38                                                                        20-07 150 10                                                                    250 35                                                                         350 73                                                                      ______________________________________                                    

Glyphosate activity on CHEAL was very weak in this test and no definitive conclusions can be drawn. However, none of the compositions of the invention performed as well as the commercial standard Formulation C in this test. Fluorad FC-135 at the extremely low concentration of 0.05% was ineffective as a tank-mix additive, but addition of 0.05% Fluorad FC-135 did enhance the performance of compositions containing lecithin (compare compositions 20-04 to 20-06 with 20-01 to 20-03).

Example 21

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 21a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 21a                                                        ______________________________________                                         Spray          % w/w                                                           compo- Lecithin                                                                               Fluorad Aerosol                                                                              Methyl                                                                               Components                                    sition g/l FC-135 OT caprate sonicated with lecithin                         ______________________________________                                         21-01  2.5                         none                                          21-02 2.5    glyphosate                                                        21-03 1.0    none                                                              21-04 1.0    glyphosate                                                        21-05 0.5    none                                                              21-06 0.5    glyphosate                                                        21-07 0.2    none                                                              21-08 0.2    glyphosate                                                        21-09 0.5  0.05  none                                                          21-10 0.5  0.05  AOT, glyphosate                                               21-11 0.5  0..05  AOT                                                          21-12 2.5 0.25   none                                                          21-13 0.5 0.05   none                                                          21-14 0.5 0.05   glyphosate                                                    21-15 0.5   0.05 Me caprate                                                    21-16 0.5 0.05  0.05 Me caprate                                                21-17 0.2 0.02   none                                                          21-18 0.2 0.02   glyphosate                                                    21-19 0.2   0.02 Me caprate                                                  ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF), and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 22 days after planting ECHCF. No record was found for the planting date for SIDSP. Evaluation of herbicidal inhibition was done 20 days after application.

In addition to compositions 21-01 to 21-19, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 21b.

                  TABLE 21b                                                        ______________________________________                                                       Glyphosate                                                         Spray rate % Inhibition                                                      composition   g a.e./ha ABUTH    ECHCF SIDSP                                   ______________________________________                                         Formulation B 150       16       23    30                                         250 17 33 57                                                                   350 24 43 65                                                                  Formulation C 150 18 58 53                                                      250 30 71 79                                                                   350 49 83 94                                                                  Formulation B + 150 27 59 56                                                   Fluorad FC-135 0.25% w/v 250 45 84 81                                           350 55 82 91                                                                  Formulation B + 150 17 43 56                                                   Fluorad FC-135 0.1% w/v 250 21 56 75                                            350 64 80 90                                                                  Formulation B + 150 22 27 38                                                   Fluorad FC-135 0.02% w/v 250 37 49 69                                           350 48 68 94                                                                  Formulation C + 150 41 41 59                                                   Fluorad FC-135 0.25% w/v 250 57 53 85                                           350 67 67 94                                                                  Formulation C + 150 26 39 67                                                   Fluorad FC-135 0.05% w/v 250 46 66 88                                           350 75 73 93                                                                  Formulation C + 150 30 52 66                                                   Fluorad FC-135 0.02% w/v 250 67 50 89                                           350 61 88 92                                                                  21-01 150 35 62 64                                                              250 63 77 90                                                                   350 71 83 85                                                                  21-02 150 35 44 67                                                              250 53 79 86                                                                   350 58 92 90                                                                  21-03 150 37 50 71                                                              250 53 76 90                                                                   350 73 63 97                                                                  21-04 150 29 46 61                                                              250 43 77 85                                                                   350 70 85 96                                                                  21-05 150 12 36 59                                                              250 43 55 83                                                                   350 53 77 87                                                                  21-06 150 19 69 67                                                              250 62 47 84                                                                   350 58 60 95                                                                  21-07 150 14 59 59                                                              250 39 63 75                                                                   350 46 77 91                                                                  21-08 150 36 37 64                                                              250 38 68 82                                                                   350 47 80 79                                                                  21-09 150 8 35 27                                                               250 9 51 56                                                                    350 36 58 67                                                                  21-10 150 5 33 24                                                               250 15 73 47                                                                   350 30 66 67                                                                  21-11 150 38 49 73                                                              250 62 75 89                                                                   350 71 75 98                                                                  21-12 150 7 41 21                                                               250 18 67 38                                                                   350 30 64 61                                                                  21-13 150 39 72 65                                                              250 65 55 76                                                                   350 70 68 90                                                                  21-14 150 51 53 66                                                              250 60 82 85                                                                   350 65 83 95                                                                  21-15 150 15 59 61                                                              250 31 54 83                                                                   350 57 67 84                                                                  21-16 150 36 79 66                                                              250 50 60 95                                                                   350 71 95 95                                                                  21-17 150 30 52 75                                                              250 54 60 84                                                                   350 48 84 93                                                                  21-18 150 43 75 69                                                              250 47 78 88                                                                   350 missing missing 90                                                        21-19 150 13 42 61                                                              250 29 51 79                                                                   350 42 69 90                                                                ______________________________________                                    

In this test the concentration of Fluorad FC-135 which had to be added in tank-mix to Formulation B to bring its herbicidal performance up to that of Formulation C was approximately 0.25% for ECHCF, 0.1% for SIDSP and 0.02% for ABUTH. The herbicidal effectiveness of composition 21-12 (0.25% lecithin, 0.25% Fluorad FC-135) was uncharacteristically weak in this test. However, composition 21-13 (0.05% lecithin, 0.05% Fluorad FC-135) performed well as in previous tests, exceeding the herbicidal effectiveness of Formulation C on ABUTH, at least equaling it on SIDSP and not quite equaling it on ECHCF. Contrary to results obtained in other tests, improved effectiveness on ECHCF and SIDSP was obtained by sonicating the glyphosate with the lecithin (composition 21-14 versus 21-13). The inclusion of methyl caprate (compositions 21-15 and 21-16) also improved efficacy on these species. Surprisingly high herbicidal effectiveness was seen in this test with compositions containing ultra-low concentrations of lecithin and Fluorad FC-135 (0.02% of each, 21-17 and 21-18).

Example 22

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 22a. Process (iv) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of these compositions was not recorded.

                  TABLE 22a                                                        ______________________________________                                                % w/w                                                                   Concentrate                                                                             Glyphosate                  Fluorad                                     composition a.e. Lecithin MON 0818 FC-135                                    ______________________________________                                         22-01    10                          5.0                                         22-02 10   10.0                                                                22-03 10   12.5                                                                22-04 10   15.0                                                                22-05 10   20.0                                                                22-06 10   30.0                                                                22-07 15 4.0 1.0                                                               22-08 20 5.0 0.5                                                               22-09 20 5.0 1.0                                                               22-10 20 5.0 2.0                                                               22-11 20 4.0 1.0                                                               22-12 25 5.0 0.5                                                               22-13 25 5.0 1.0                                                               22-14 25 5.0 2.0                                                               22-15 25 4.0 1.0                                                               22-16 25 5.0 5.0                                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and 16 days after planting ECHCF, and evaluation of herbicidal inhibition was done 14 days after application.

Formulation C was applied as a comparative treatment. Results, averaged for all replicates of each treatment, are shown in Table 22b.

                  TABLE 22b                                                        ______________________________________                                                      Glyphosate rate                                                                              % Inhibition                                        Concentrate composition                                                                       g a.e./ha  ABUTH      ECHCF                                     ______________________________________                                         Formulation C  56         13         45                                           112 43 75                                                                      224 64 94                                                                      448 88 97                                                                     22-01 112 38 61                                                                 224 56 80                                                                      448 76 97                                                                     22-02 112 50 51                                                                 224 69 91                                                                      448 81 97                                                                     22-03 112 51 63                                                                 224 64 83                                                                      448 81 96                                                                     22-04 112 53 61                                                                 224 71 91                                                                      448 78 95                                                                     22-05 112 41 56                                                                 224 70 85                                                                      448 75 97                                                                     22-06 112 38 53                                                                 224 63 89                                                                      448 75 94                                                                     22-07 112 48 53                                                                 224 49 84                                                                      448 75 90                                                                     22-08 112 31 60                                                                 224 53 84                                                                      448 66 90                                                                     22-09 112 26 56                                                                 224 53 85                                                                      448 78 96                                                                     22-10 112 36 60                                                                 224 53 85                                                                      448 79 98                                                                     22-11 112 41 59                                                                 224 49 73                                                                      448 76 95                                                                     22-12 112 30 56                                                                 224 50 74                                                                      448 65 89                                                                     22-13 112 34 55                                                                 224 44 80                                                                      448 73 95                                                                     22-14 112 39 61                                                                 224 56 85                                                                      448 69 91                                                                     22-15 112 31 55                                                                 224 56 69                                                                      448 79 95                                                                     22-16 112 29 64                                                                 224 58 86                                                                      448 78 91                                                                   ______________________________________                                    

None of the concentrate compositions of this Example containing 10% glyphosate a.e. and varying amounts of Fluorad FC-135 (22-01 to 22-06) exhibited greater herbicidal effectiveness than the commercial standard Formulation C. It should be noted that the amounts of Fluorad FC-135 used in this Example were extremely high, the weight/weight ratio of Fluorad FC-135 to glyphosate a.e. ranging from 1:2 to 3:1.

Example 23

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 23a. Process (iv) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 23a                                                        ______________________________________                                         % w/w                      Components                                          Concentrate                                                                            Glyphosate        MON    Fluorad                                                                              sonicated                                 composition a.e. Lecithin 0818 FC-135 with lecithin                          ______________________________________                                         23-01   20        5.0     2.0          none                                      23-02 20 4.0 1.0  none                                                         23-03 20 5.0 2.0  glyphosate                                                   23-04 20 4.0 1.0  glyphosate                                                   23-05 20 5.0 2.0 5.0 none                                                    ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and 18 days after planting ECHCF, and evaluation of herbicidal inhibition was done 14 days after application.

Formulations B and C were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 23b.

                  TABLE 23b                                                        ______________________________________                                                      Glyphosate rate                                                                              % Inhibition                                        Concentrate composition                                                                       g a.e./ha  ABUTH      ECHCF                                     ______________________________________                                         Formulation B  112        33         53                                           224 58 78                                                                      336 80 89                                                                      448 79 88                                                                     Formulation C 112 49 79                                                         224 59 94                                                                      336 84 100                                                                     448 95 100                                                                    23-01 112 39 66                                                                 224 63 93                                                                      336 81 98                                                                      448 86 100                                                                    23-02 112 29 46                                                                 224 55 83                                                                      336 79 91                                                                      448 85 95                                                                     23-03 112 30 59                                                                 224 60 98                                                                      336 80 100                                                                     448 81 100                                                                    23-04 112 26 51                                                                 224 53 83                                                                      336 76 86                                                                      448 86 99                                                                     23-05 112 46 51                                                                 224 59 89                                                                      336 79 96                                                                      448 89 98                                                                   ______________________________________                                    

Concentrate composition 23-05 (5% lecithin, 2% MON 0818, 5% Fluorad FC-135) did not exhibit greater herbicidal effectiveness in this test than composition 23-01 lacking the Fluorad FC-135.

Example 24

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 24a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of these compositions was not recorded.

                  TABLE 24a                                                        ______________________________________                                         Spray    Lecithin                                                                               % w/w         Components                                        composition g/l Fluorad FC-135 sonicated with lecithin                       ______________________________________                                         24-01    2.5                   none                                              24-02 1.0  none                                                                24-03 0.5  none                                                                24-04 0.2  none                                                                24-05 0.1  none                                                                24-06 2.5 0.25 none                                                            24-07 0.5 0.05 none                                                            24-08 0.2 0.02 none                                                            24-09 0.2 0.02 glyphosate                                                      24-10 0.2 0.02 FC-135                                                          24-11 0.1 0.01 none                                                            24-12 0.1 0.01 glyphosate                                                      24-13 0.1 0.02 FC-135                                                          24-14 0.5 0.02 none                                                            24-15 0.5 0.02 glyphosate                                                      24-16 0.5 0.02 FC-135                                                        ______________________________________                                    

Yellow nutsedge (Cyperus esculentus, CYPES) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 29 days after planting, and evaluation of herbicidal inhibition was done 33 days after application.

In addition to compositions 24-01 to 24-16, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 24b.

                  TABLE 24b                                                        ______________________________________                                                          Glyphosate rate                                                                           % Inhibition                                         Spray composition g a.e./ha CYPES                                            ______________________________________                                         Formulation B    400        32                                                    750 68                                                                         1000 70                                                                       Formulation C 400 25                                                            750 66                                                                         1000 89                                                                       Formulation B + 400 49                                                         Fluorad FC-135 0.25% w/v 750 75                                                 1000 82                                                                       Formulation B + 400 53                                                         Fluorad FC-135 0.05% w/v 750 74                                                 1000 64                                                                       Formulation B + 400 56                                                         Fluorad FC-135 0.02% w/v 750 83                                                 1000 83                                                                       Formulation B + 400 61                                                         Fluorad FC-135 0.01% w/v 750 67                                                 1000 88                                                                       Formulation C + 400 73                                                         Fluorad FC-135 0.25% w/v 750 47                                                 1000 79                                                                       Formulation C + 400 50                                                         Fluorad FC-135 0.05% w/v 750 73                                                 1000 81                                                                       Formulation C + 400 41                                                         Fluorad FC-135 0.02% w/v 750 79                                                 1000 81                                                                       Formulation C + 400 67                                                         Fluorad FC-135 0.01% w/v 750 77                                                 1000 72                                                                       24-01 400 62                                                                    750 73                                                                         1000 100                                                                      24-02 400 61                                                                    750 85                                                                         1000 92                                                                       24-03 400 81                                                                    750 83                                                                         1000 87                                                                       24-04 400 59                                                                    750 79                                                                         1000 79                                                                       24-05 400 69                                                                    750 69                                                                         1000 91                                                                       24-06 400 75                                                                    750 80                                                                         1000 96                                                                       24-07 400 65                                                                    750 69                                                                         1000 89                                                                       24-08 400 67                                                                    750 69                                                                         1000 87                                                                       24-09 400 76                                                                    750 77                                                                         1000 80                                                                       24-10 400 71                                                                    750 75                                                                         1000 86                                                                       24-11 400 69                                                                    750 77                                                                         1000 85                                                                       24-12 400 59                                                                    750 85                                                                         1000 95                                                                       24-13 400 61                                                                    750 75                                                                         1000 81                                                                       24-14 400 64                                                                    750 83                                                                         1000 90                                                                       24-15 400 53                                                                    750 81                                                                         1000 86                                                                       24-16 400 85                                                                    750 86                                                                         1000 81                                                                     ______________________________________                                    

The tank-mix treatments of this Example show surprisingly little effect on herbicidal effectiveness on CYPES of reducing Fluorad FC-135 concentration from 0.25% all the way down to 0.01%. At this extraordinarily low concentration, the tank mix of Formulation B with Fluorad FC-135 still performed equal or better than Formulation C alone. Lecithin alone was an unexpectedly effective excipient for glyphosate in this test (see compositions 24-01 to 24-05) and the addition of Fluorad FC-135 to lecithin did not in every case give further enhancement of herbicidal efficacy.

Example 25

Glyphosate-containing spray compositions were prepared by tank-mixing Formulation B with excipients as shown in Table 25. Soybean lecithin (20% phospholipid, Avanti) was used in the form of a 10% dispersion prepared by sonication as in process (iii).

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 21 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 21 days after application. Results, averaged for all replicates of each treatment, are shown in Table 25.

                                      TABLE 25                                     __________________________________________________________________________     Glyphosate                                                                            Glyphosate rate                                                                               Add. rate                                                                           % Inhibition                                        composition                                                                           g a.e./ha                                                                             Additive                                                                               % w/v                                                                               ABUTH                                                                               ECHCF                                          __________________________________________________________________________     Formulation B                                                                         56                  3    17                                                112   7 38                                                                     224   30 58                                                                    336   60 67                                                                   None 0 MON 0818 5.0 7 30                                                         Fluorad FC-135 5.0 5 3                                                         lecithin 5.0 0 0                                                             Formulation B 56 MON 0818 0.005 0 48                                            112   3 60                                                                     224   53 85                                                                    336   58 87                                                                   Formulation B 56 MON 0818 0.01 3 50                                             112   10 67                                                                    224   52 87                                                                    336   67 92                                                                   Formulation B 56 MON 0818 0.05 7 52                                             112   10 67                                                                    224   60 93                                                                    336   68 96                                                                   Formulation B 56 MON 0818 0.1 10 55                                             112   12 70                                                                    224   57 97                                                                    336   80 97                                                                   Formulation B 56 MON 0818 0.2 10 65                                             112   22 70                                                                    224   58 97                                                                    336   85 97                                                                   Formulation B 56 MON 0818 0.5 13 65                                             112   33 77                                                                    224   72 99                                                                    336   88 100                                                                  Formulation B 56 MON 0818 1.0 15 68                                             112   55 80                                                                    224   78 98                                                                    336   95 100                                                                  Formulation B 56 MON 0818 2.0 27 75                                             112   62 78                                                                    224   83 100                                                                   336   100 99                                                                  Formulation B 56 MON 0818 5.0 23 55                                             112   53 77                                                                    224   72 90                                                                    336   97 88                                                                   Formulation B 56 Fluorad FC-135 0.005 2 47                                      112   10 50                                                                    224   25 70                                                                    336   55 78                                                                   Formulation B 56 Fluorad FC-135 0.01 7 40                                       112   15 57                                                                    224   70 67                                                                    336   80 80                                                                   Formulation B 56 Fluorad FC-135 0.05 2 48                                       112   15 57                                                                    224   70 78                                                                    336   78 88                                                                   Formulation B 56 Fluorad FC-135 0.1 5 45                                        112   18 58                                                                    224   75 87                                                                    336   80 90                                                                   Formulation B 56 Fluorad FC-135 0.2 12 48                                       112   27 60                                                                    224   75 90                                                                    336   97 93                                                                   Formulation B 56 Fluorad FC-135 0.5 3 47                                        112   12 57                                                                    224   75 80                                                                    336   78 83                                                                   Formulation B 56 Fluorad FC-135 1.0 5 43                                        112   10 52                                                                    224   77 75                                                                    336   78 77                                                                   Formulation B 56 Fluorad FC-135 2.0 7 42                                        112   10 47                                                                    224   65 65                                                                    336   72 77                                                                   Formulation B 56 Fluorad FC-135 5.0 2 38                                        112   5 47                                                                     224   63 60                                                                    336   67 63                                                                   Formulation B 56 lecithin 0.005 0 10                                            112   10 45                                                                    224   67 70                                                                    336   67 77                                                                   Formulation B 56 lecithin 0.01 2 20                                             112   12 47                                                                    224   63 70                                                                    336   68 85                                                                   Formulation B 56 lecithin 0.05 3 32                                             112   12 52                                                                    224   63 73                                                                    336   72 82                                                                   Formulation B 56 lecithin 0.1 8 37                                              112   10 50                                                                    224   65 73                                                                    336   78 83                                                                   Formulation B 56 lecithin 0.2 5 45                                              112   43 63                                                                    224   68 82                                                                    336   80 92                                                                   Formulation B 56 lecithin 0.5 13 50                                             112   42 65                                                                    224   67 88                                                                    336   68 87                                                                   Formulation B 56 lecithin 1.0 13 52                                             112   50 72                                                                    224   67 80                                                                    336   68 88                                                                   Formulation B 56 lecithin 2.0 10 53                                             112   37 72                                                                    224   72 88                                                                    336   87 97                                                                   Formulation B 56 lecithin 5.0 10 50                                             112   55 73                                                                    224   72 80                                                                    336   78 95                                                                 __________________________________________________________________________

This test was an expanded rate titration study of MON 0818, Fluorad FC-135 and lecithin as tank-mix adjuvants for glyphosate as Formulation B. On ABUTH, the optimum adjuvant concentration was 2.0% for MON 0818, 0.2% for Fluorad FC-135 and 0.2% or higher for lecithin. On ECHCF, the optimum adjuvant concentration was 0.5% to 2.0% for MON 0818, 0.2% for Fluorad FC-135 and 2.0% for lecithin.

Example 26

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 26a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 26a                                                        ______________________________________                                         Spray     Lecithin  % w/v                                                      composition                                                                              g/l       Fluorad FC-135                                                                             Aerosol OT                                     ______________________________________                                         26-01                           0.1                                              26-02   0.05                                                                   26-03   0.02                                                                   26-04  0.1 0.1                                                                 26-05  0.05 0.05                                                               26-06  0.02 0.02                                                               26-07 1.0  0.10                                                                26-08 1.0 0.10 0.10                                                            26-09 1.0                                                                      26-10 1.0 0.10                                                                 26-11 0.5                                                                      26-12 0.5  0.05                                                                26-13 0.5 0.05                                                                 26-14 0.5 0.05 0.05                                                            26-15 0.2                                                                      26-16 0.2  0.02                                                                26-17 0.2 0.02                                                                 26-18 0.2 0.02 0.02                                                          ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH, 19 days after planting ECHCF, and 26 days after planting SIDSP. Evaluation of herbicidal inhibition was done for ABUTH and ECHCF 15 days after application and for SIDSP 21 days after application.

In addition to compositions 26-01 to 26-18, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 26b.

                  TABLE 26b                                                        ______________________________________                                                     Glyphosate                                                           rate % Inhibition                                                            Spray composition                                                                            g a.e./ha ABUTH    ECHCF SIDSP                                   ______________________________________                                         Formulation B 150       37       71    57                                         250 57 79 69                                                                   400 74 86 80                                                                   500 79 89 74                                                                  Formulation C 150 48 42 58                                                      250 71 80 81                                                                   400 88 100 88                                                                  500 92 100 86                                                                 Formulation B + 150 87 62 66                                                   Fluorad FC-135 0.1% w/v 250 87 96 70                                            400 91 94 75                                                                  Formulation B + 150 61 48 65                                                   Fluorad FC-135 0.05% w/v 250 81 69 71                                           400 90 91 67                                                                  Formulation B + 150 58 32 62                                                   Fluorad FC-135 0.02% w/v 250 75 49 51                                           400 81 83 73                                                                  Formulation C + 150 78 61 76                                                   Fluorad FC-135 0.1% w/v 250 79 77 81                                            400 93 100 78                                                                 Formulation C + 150 43 86 69                                                   Fluorad FC-135 0.05% w/v 250 79 100 80                                          400 95 98 84                                                                  Formulation C + 150 39 56 77                                                   Fluorad FC-135 0.02% w/v 250 77 100 86                                          400 88 100 80                                                                 26-01 150 63 48 49                                                              250 70 69 66                                                                   400 85 84 63                                                                  26-02 150 32 36 55                                                              250 64 74 65                                                                   400 77 92 69                                                                  26-03 150 30 78 51                                                              250 59 79 66                                                                   400 83 93 74                                                                  26-04 150 86 50 65                                                              250 74 98 71                                                                   400 81 89 75                                                                  26-05 150 85 55 60                                                              250 81 75 73                                                                   400 82 81 64                                                                  26-06 150 61 67 45                                                              250 66 78 61                                                                   400 83 77 67                                                                  26-07 150 46 38 44                                                              250 56 85 64                                                                   400 75 96 78                                                                  26-08 150 88 63 70                                                              250 87 73 79                                                                   400 91 82 75                                                                  26-09 150 63 72 61                                                              250 87 73 71                                                                   400 89 87 80                                                                  26-10 150 81 72 61                                                              250 85 62 82                                                                   400 87 89 76                                                                  26-11 150 54 57 68                                                              250 80 90 74                                                                   400 84 95 66                                                                  26-12 150 27 53 47                                                              250 57 71 67                                                                   400 72 91 70                                                                  26-13 150 78 59 64                                                              250 80 84 80                                                                   400 89 76 77                                                                  26-14 150 84 52 68                                                              250 88 69 75                                                                   400 90 84 66                                                                  26-15 150 51 57 55                                                              250 81 55 71                                                                   400 88 83 69                                                                  26-16 150 40 68 46                                                              250 74 89 60                                                                   400 77 98 63                                                                  26-17 150 64 44 58                                                              250 80 93 81                                                                   400 87 99 69                                                                  26-18 150 64 87 50                                                              250 77 75 70                                                                   400 90 89 50                                                                ______________________________________                                    

This test was designed in part to explore the relative contribution of Fluorad FC-135 and lecithin to the herbicidal effectiveness of glyphosate compositions comprising both of these excipient substances. Fluorad FC-135 was applied as sole excipient at concentrations of 1.0%, 0.5% and 0.2% (see tank-mix treatments with Formulation B). Lecithin was applied as sole excipient at the same three concentrations in compositions 26-09, 26-11 and 26-15. Combinations of the two excipients at equal concentrations were applied in corresponding compositions 26-10, 26-13 and 26-17. The data are highly variable but an overall trend can be discerned. When only one of the two excipients was present, herbicidal effectiveness tended to drop off as the concentration of that excipient was reduced. When both excipients were present, there was scarcely any decline in herbicidal effectiveness as excipient concentration was reduced. Although averages of data from three glyphosate rates across three species can be misleading, it is helpful in this case to reduce the mass of individual data to the following such averages of percent inhibition:

Glyphosate (Formulation B) 68%

Glyphosate +0.1% Fluorad FC-135 81%

Glyphosate +0.05% Fluorad FC-135 71%

Glyphosate +0.02% Fluorad FC-135 63%

Glyphosate +0.1% lecithin 76%

Glyphosate +0.05% lecithin 74%

Glyphosate +0.02% lecithin 68%

Glyphosate +0.1% Fluorad FC-135+0.1% lecithin 77%

Glyphosate +0.05% Fluorad FC-135+0.05% lecithin 76%

Glyphosate +0.02% Fluorad FC-135+0.02% lecithin 75%

Glyphosate commercial standard (Formulation C) 73%

Thus, when both excipients arc used together, a fivefold decrease in excipient concentration results in a decline in overall herbicidal effectiveness of only 2 percentage points, still retaining overall effectiveness at least equal to that of the commercial standard.

Example 27

Glyphosate-containing spray compositions were prepared by tank-mixing Formulations B with excipients as shown in Table 27. Soybean lecithin (20% phospholipid, Avanti) was used in the form of a 10% dispersion prepared by sonication as in process (iii).

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 15 days after planting ECHCF, and evaluation of herbicidal inhibition was done 19 days after application. Results, averaged for all replicates of each treatment, are shown in Table 27.

                                      TABLE 27                                     __________________________________________________________________________     Glyphosate                                                                            Glyphosate rate   Additive rate                                                                         % Inhibition                                   composition                                                                           g a.e./ha                                                                             Additive   % v/v  ABUTH                                                                               ECHCF                                     __________________________________________________________________________     Formulation B                                                                         56     none              0    3                                            112   5 13                                                                     224   40 40                                                                    336   83 77                                                                   Formulation B 56 Fluorad FC-135 0.005 0 7                                       112   3 10                                                                     224   45 53                                                                    336   58 78                                                                   Formulation B 56 Fluorad FC-135 0.01 0 g                                        112   2 12                                                                     224   45 60                                                                    336   67 87                                                                   Formulation B 56 Fluorad FC-135 0.05 2 8                                        112   20 23                                                                    224   72 88                                                                    336   90 93                                                                   Formulation B 56 Fluorad FC-135 0.1 3 10                                        112   33 38                                                                    224   73 88                                                                    336   93 92                                                                   Formulation B 56 Fluorad FC-135 0.2 10 17                                       112   33 47                                                                    224   77 85                                                                    336   93 92                                                                   Formulation B 56 Fluorad FC-135 0.5 7 13                                        112   37 37                                                                    224   80 85                                                                    336   96 95                                                                   Formulation B 56 Fluorad FC-135 1.0 3 7                                         112   27 35                                                                    224   72 87                                                                    336   88 92                                                                   Formulation B 56 Fluorad FC-135 2.0 0 0                                         112   27 18                                                                    224   72 75                                                                    336   87 87                                                                   Formulation B 56 Fluorad FC-135 5.0 0 0                                         112   12 13                                                                    224   43 50                                                                    336   58 53                                                                   Formulation B 56 lecithin/FC-135 (1:1) 0.005 0 2                                112   7 13                                                                     224   65 63                                                                    336   83 82                                                                   Formulation B 56 lecithin/FC-135 (1:1) 0.01 0 0                                 112   3 10                                                                     224   42 63                                                                    336   73 82                                                                   Formulation B 56 lecithin/FC-135 (1:1) 0.05 0 0                                 112   42 13                                                                    224   68 73                                                                    336   98 73                                                                   Formulation B 56 leeithin/FC-135 (1:1) 0.1 0 0                                  112   37 20                                                                    224   62 68                                                                    336   94 77                                                                   Formulation B 56 lecithin/FC-135 (1:1) 0.2 0 2                                  112   33 28                                                                    224   67 68                                                                    336   100 78                                                                  Formulation B 56 lecithin/FC-135 (1:1) 0.5 7 0                                  112   40 18                                                                    224   68 68                                                                    336   90 73                                                                   Formulation B 56 lecithin/FC-135 (1:1) 1.0 17 3                                 112   43 45                                                                    224   83 88                                                                    336   95 94                                                                   Formulation B 56 lecithin/FC-135 (1:1) 2.0 10 23                                112   32 42                                                                    224   63 73                                                                    336   88 87                                                                   Formulation B 56 lecithin/FC-135 (1:1) 5.0 2 3                                  112   18 28                                                                    224   50 72                                                                    336   85 87                                                                   Formulation B 56 lecithin 0.005 2 2                                             112   3 10                                                                     224   45 50                                                                    336   58 72                                                                   Formulation B 56 lecithin 0.01 0 2                                              112   2 12                                                                     224   40 52                                                                    336   65 75                                                                   Formulation B 56 lecithin 0.05 2 2                                              112   0 10                                                                     224   40 45                                                                    336   57 70                                                                   Formulation B 56 lecithin 0.1 2 7                                               112   2 13                                                                     224   33 37                                                                    336   48 67                                                                   Formulation B 56 lecithin 0.2 3 3                                               112   3 13                                                                     224   32 35                                                                    336   47 68                                                                   Formulation B 56 lecithin 0.5 2 3                                               112   8 15                                                                     224   47 53                                                                    336   67 65                                                                   Formulation B 56 lecithin 1.0 2 5                                               112   10 15                                                                    224   33 55                                                                    336   70 77                                                                   Formulation B 56 lecithin 2.0 5 8                                               112   12 17                                                                    224   48 52                                                                    336   68 77                                                                   Formulation B 56 lecithin 5.0 5 17                                              112   23 17                                                                    224   52 55                                                                    336   73 78                                                                 __________________________________________________________________________

This tank-mix study more clearly demonstrates the surprising interaction seen in Example 26 between lecithin and Fluorad FC-135 as excipients for glyphosate. For example, glyphosate alone over four rates gave average inhibition of ABUTH of 32%. Adding Fluorad FC-135 at a concentration of 0.5% boosted the average inhibition to 55%, but adding lecithin at the same concentration did not raise average inhibition above 32%. A 1:1 combination of both excipients at the same total concentration gave an average inhibition of51%. At a concentration of 0.1%, Fluorad FC-135 gave average inhibition of 50%, lecithin 21% (i.e. a reduction in effectiveness of glyphosate) and the 1:1 combination 48%. Thus, as in Example 26, the decline in herbicidal effectiveness with reducing excipient rate was much less pronounced with the combination than with either excipient on its own.

Example 28

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 28a. Process (i) was followed for compositions 28-01 to 28-06. Process (iv) was followed for compositions 28-07 to 28-11, using soybean lecithin (20% phospholipid, Avanti). For compositions 28-12 and 28-13, process (iv) was also used, but Aerosol OT was the aggregate-forming material employed in place of lecithin. The pH of all compositions was approximately 5.

                  TABLE 28a                                                        ______________________________________                                         Concen-                                                                          trate % w/w                                                                  compo- Glyphosate        Fluorad                                                                              MON  Other                                                                               (*) Other                               sition a.e. Lecithin FC-135 0818 (*) components                              ______________________________________                                         28-01  20                           1.0  PVA                                     28-02 20  5.0  1.0 PVA                                                         28-03 20  2.0  1.0 PVA                                                         28-04 20  1.0  1.0 PVA                                                         28-05 20    0.5 Kelzan                                                         28-06 20  2.0  0.5 Kelzan                                                      28-07 20 2.0  0.04                                                             28-08 20 2.0 2.0 0.04                                                          28-09 20 2.0 2.0 0.02                                                          28-10 20 2.0  0.04 25.0  Silwet 800                                            28-11 20 2.0 2.0 0.04 25.0  Silwet 800                                         28-12 20    5.0 Aerosol OT                                                     28-13 20    5.0 + Aerosol                                                           25.0 OT +                                                                       Silwet 800                                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and 17 days after planting ECHCF, and evaluation of herbicidal inhibition was done 38 days after application.

Formulations B and C, were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 28b.

                  TABLE 28b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B  56          0         8                                            112  4 33                                                                      224 45 40                                                                      336 69 65                                                                     Formulation C  56  0 10                                                         112  5 43                                                                      224 68 73                                                                      336 87 94                                                                     28-01 112  0 40                                                                 224 50 76                                                                      336 76 85                                                                     28-02 112  1 35                                                                 224 30 70                                                                      336 69 96                                                                     28-03 112  6 35                                                                 224 35 58                                                                      336 65 84                                                                     28-04 112  1 35                                                                 224 70 60                                                                      336 69 85                                                                     28-05 112  1 35                                                                 224 63 68                                                                      336 80 88                                                                     28-06 112  0 25                                                                 224 40 55                                                                      336 66 73                                                                     28-07 112 11 35                                                                 224 45 68                                                                      336 65 86                                                                     28-08 112  9 38                                                                 224 65 60                                                                      336 66 75                                                                     28-09 112 10 33                                                                 224 56 60                                                                      336 78 75                                                                     28-10 112 30  5                                                                 224 79 30                                                                      336 90 35                                                                     28-11 112 60  5                                                                 224 79 33                                                                      336 96 30                                                                     28-12 112  8 11                                                                 224 53 40                                                                      336 66 64                                                                     28-13 112 40  6                                                                 224 91 33                                                                      336 98 38                                                                   ______________________________________                                    

Concentrate compositions 28-08 and 28-09 did not in this test exhibit herbicidal effectiveness equal to Formulation C.

Example 29

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 29a. Process (iii) was followed for all compositions, using soybean lecithin (20% or 45% phospholipid as indicated below, both sourced from Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 29a                                                        ______________________________________                                         Spray       Lecithin       % w/w                                               composition g/l     phospholipid %                                                                            Fluorad FC-135                                  ______________________________________                                         29-01       0.25    20                                                           29-02 0.05 20                                                                  29-03 0.02 20                                                                  29-04 0.01 20                                                                  29-05 0.25 20 0.25                                                             29-06 0.05 20 0.05                                                             29-07 0.02 20 0.02                                                             29-08 0.01 20 0.01                                                             29-09 0.25 45                                                                  29-10 0.05 45                                                                  29-11 0.02 45                                                                  29-12 0.01 45                                                                  29-13 0.25 45 0.25                                                             29-14 0.05 45 0.05                                                             29-15 0.02 45 0.02                                                             29-16 0.01 45 0.01                                                           ______________________________________                                    

Yellow nutsedge (Cyperus esculentus, CYPES) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 27 days after planting CYPES. Evaluation was done 27 days after application.

In addition to compositions 29-01 to 29-16, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 29b.

                  TABLE 29b                                                        ______________________________________                                                          Glyphosate rate                                                                           % Inhibition                                         Spray Composition g a.e./ha CYPBS                                            ______________________________________                                         Formulation B    500        25                                                    800 41                                                                         1200  59                                                                      Formulation C 500 29                                                            800 43                                                                         1200  62                                                                      Formulation B + 500 60                                                         Fluorad FC-135 0.25% w/v 800 57                                                 1200  79                                                                      Formulation B + 500 63                                                         Fluorad FC-135 0.05% w/v 800 54                                                 1200  65                                                                      Formulation B + 500 50                                                         Fluorad FC-135 0.02% w/v 800 71                                                 1200  60                                                                      Formulation B + 500 27                                                         Fluorad FC-135 0.01% w/v 800 35                                                 1200  81                                                                      Formulation C + 500 41                                                         Fluorad FC-135 0.25% w/v 800 72                                                 1200  75                                                                      Formulation C + 500 52                                                         Fluorad FC-135 0.05% w/v 800 43                                                 1200  63                                                                      Formulation C + 500 76                                                         Fluorad FC-135 0.02% w/v 800 72                                                 1200  82                                                                      Formulation C + 500 38                                                         Fluorad FC-135 0.01% w/v 800 59                                                 1200  72                                                                      29-01 500 51                                                                    800 70                                                                         1200  64                                                                      29-02 500 58                                                                    800 69                                                                         1200  77                                                                      29-03 500 49                                                                    800 67                                                                         1200  85                                                                      29-04 500 51                                                                    800 76                                                                         1200  77                                                                      29-05 500 37                                                                    800 73                                                                         1200  100                                                                     29-06 400 72                                                                    750 62                                                                         1000  67                                                                      29-07 400 68                                                                    750 75                                                                         1000  86                                                                      29-08 400 59                                                                    750 78                                                                         1000  88                                                                      29-09 400 72                                                                    750 80                                                                         1000  88                                                                      29-10 400 67                                                                    750 77                                                                         1000  89                                                                      29-11 400 67                                                                    750 75                                                                         1000  66                                                                      29-12 400 55                                                                    750 75                                                                         1000  83                                                                      29-13 400 33                                                                    750 59                                                                         1000  73                                                                      29-14 400 63                                                                    750 77                                                                         1000  76                                                                      29-15 400 35                                                                    750 75                                                                         1000  88                                                                      29-16 400 77                                                                    750 66                                                                         1000  86                                                                    ______________________________________                                    

This test was conducted to investigate the effect of phospholipid content of lecithin on herbicidal efficacy of lecithin-containing glyphosate compositions. No clear pattern emerged from this study, but overall it appeared that the crude lecithin (20% phospholipid) provided greater herbicidal effectiveness on CYPES than the de-oiled lecithin (45% phospholipid), suggesting that the oil present in crude lecithin might be having an adjuvant effect on this species.

Example 30

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 30a. Process (iii) was followed for all compositions, using soybean lecithin (20%, 45% or 95% phospholipid as indicated below, all sourced from Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 30a                                                        ______________________________________                                         Spray           Lecithin       % w/w                                           composition                                                                              g/l       phospholipid %                                                                            Fluorad FC-135                                  ______________________________________                                         30-01     0.5       20                                                           30-02 0.2 20                                                                   30-03 0.1 20                                                                   30-04 0.5 45                                                                   30-05 0.2 45                                                                   30-06 0.1 45                                                                   30-07 0.5 95                                                                   30-08 0.2 95                                                                   30-09 0.1 95                                                                   30-10 0.5 20 0.05                                                              30-11 0.5 45 0.05                                                              30-12 0.5 95 0.05                                                              30-13 0.2 20 0.02                                                              30-14 0.2 45 0.02                                                              30-15 0.2 95 0.02                                                              30-16 0.1 20 0.01                                                              30-17 0.1 45 0.01                                                              30-18 0.1 95 0.01                                                            ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH, 19 days after planting ECHCF, and 23 days after planting SIDSP. Evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 30-01 to 30-18, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 30b.

                  TABLE 30b                                                        ______________________________________                                                     Glyphosate                                                           rate % Inhibition                                                            Spray composition                                                                            g a.e./ha ABUTH    ECHCF SIDSP                                   ______________________________________                                         Formulation B 100       10       25    33                                         200 22 29 49                                                                   300 50 62 61                                                                   400 62 62 64                                                                  Formulation C 100 14 40 34                                                      200 53 98 66                                                                   300 74 100  84                                                                 400 86 100  93                                                                Formulation B + 100 18 25 34                                                   Fluorad FC-135 0.05% w/v 200 50 58 52                                           300 68 83 70                                                                  Formulation B + 100 10 21 29                                                   Fluorad FC-135 0.02% w/v 200 64 40 46                                           300 79 62 64                                                                  Formulation B + 100 10 21 34                                                   Fluorad FC-135 0.01% w/v 200 34 27 44                                           300 73 74 69                                                                  Formulation C + 100 65 53 58                                                   Fluorad FC-135 0.05% w/v 200 73 77 65                                           300 94 99 73                                                                  Formulation C + 100 68 94 61                                                   Fluorad FC-135 0.02% w/v 200 63 93 66                                           300 85 90 79                                                                  Formulation C + 100 72 67 53                                                   Fluorad FC-135 0.01% w/v 200 69 99 61                                           300 81 99 83                                                                  30-01 100 32 26 39                                                              200 72 60 56                                                                   300 84 72 69                                                                  30-02 100 14 23 43                                                              200 70 42 63                                                                   300 83 74 68                                                                  30-03 100  6 25 42                                                              200 55 47 57                                                                   300 65 64 72                                                                  30-04 100 29 31 42                                                              200 55 65 60                                                                   300 82 54 73                                                                  30-05 100 14 22 41                                                              200 32 35 66                                                                   300 81 98 70                                                                  30-06 100  9 26 29                                                              200 47 48 57                                                                   300 69 71 71                                                                  30-07 100 30 22 50                                                              200 73 50 69                                                                   300 82 86 67                                                                  30-08 100 41 23 53                                                              200 57 38 69                                                                   300 76 46 84                                                                  30-09 100 32 17 45                                                              200 60 37 67                                                                   300 78 77 73                                                                  30-10 100 58 27 62                                                              200 91 42 79                                                                   300 93 95 77                                                                  30-11 100 66 58 63                                                              200 91 79 69                                                                   300 91 84 84                                                                  30-12 100 61 27 67                                                              200 90 72 77                                                                   300 93 83 84                                                                  30-13 100 61 24 51                                                              200 88 48 69                                                                   300 94 54 75                                                                  30-14 100 66 25 56                                                              200 90 49 72                                                                   300 93 73 85                                                                  30-15 100 63 23 61                                                              200 88 33 72                                                                   300 95 75 81                                                                  30-16 100 75 25 56                                                              200 87 37 74                                                                   300 93 71 77                                                                  30-17 100 63 17 59                                                              200 92 27 73                                                                   300 92 83 78                                                                  30-18 100 67 22 53                                                              200 91 38 68                                                                   300 91 46 77                                                                ______________________________________                                    

In general, across the three species included in this test, compositions containing the 45% phospholipid grade of soybean lecithin provided slightly greater herbicidal effectiveness than those containing the 20% grade. Any further improvement obtained by using the 95% grade was minimal and would likely not justify the considerably increased cost of this grade. The data of this test clearly show a non-additive interaction between lecithin and Fluorad FC-135. To take just one example for illustration, glyphosate alone (Formulation B) at 200 g a.e./ha gave 22% inhibition of ABUTH, 29% inhibition of ECHCF and 49% inhibition of SIDSP. Adding 0.02% Fluorad FC-135 brought these percentage inhibitions to 64%, 40% and 46% respectively. Alternatively, adding the 45% grade of lecithin at 0.02% (composition 30-05) resulted in percentage inhibitions of 32%, 35% and 36% respectively. Adding both these excipients, each at 0.02% (composition 30-14) gave percentage inhibitions of 90%, 49% and 72% respectively. Even adding both excipients so that the total excipient concentration was 0.02% (composition 30-17) resulted in percentage inhibitions of 92%, 27% and 73% respectively. Thus at least on the broadleaf species (ABUTH and SIDSP) there is strong evidence of a synergistic interaction between these two excipient substances.

Example 31

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 31a. Process (iii) was followed for all compositions, using lecithin (20% or 95% phospholipid from soybean, or 95% phospholipid from egg yolk, all sourced from Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 31a                                                        ______________________________________                                         Lecithin               % w/w                                                   Spray           phospho-         Fluorad                                                                               Fluorad                                  composition g/l lipid % source FC-135 FC-754                                 ______________________________________                                         31-01   0.05    95       egg yolk                                                31-02 0.02 95 egg yolk                                                         31-03 0.01 95 egg yolk                                                         31-04 0.05 95 soybean                                                          31-05 0.02 95 soybean                                                          31-06 0.01 95 soybean                                                          31-07 0.05 95 egg yolk 0.05                                                    31-08 0.02 95 egg yolk 0.02                                                    31-09 0.01 95 egg yolk 0.01                                                    31-10 0.05 95 soybean 0.05                                                     31-11 0.02 95 soybean 0.02                                                     31-12 0.01 95 soybean 0.01                                                     31-13 0.05 20 soybean  0.05                                                    31-14 0.02 20 soybean  0.02                                                  ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 19 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 31-01 to 31-14, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 or Fluorad FC-754 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 31b.

                  TABLE 31b                                                        ______________________________________                                                     Glyphosate rate                                                                           % Inhibition                                            Spray composition                                                                            g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          1        27                                            200  6 28                                                                      300 21 35                                                                      400 31 46                                                                     Formulation C 100 10 31                                                         200 28 36                                                                      300 62 66                                                                      400 77 74                                                                     Formulation B + 100 19 24                                                      Fluorad FC-135 0.05% w/v 200 37 40                                              300 62 52                                                                     Formulation B + 100  7 13                                                      Fluorad FC-135 0.02% w/v 200 42 27                                              300 56 57                                                                     Formulation B + 100 23 19                                                      Fluorad FC-135 0.01% w/v 200 43 24                                              300 60 40                                                                     Formulation B + 100 19 23                                                      Fluorad FC-754 0.05% w/v 200 41 33                                              300 67 62                                                                     Formulation B + 100 12 19                                                      Fluorad FC-754 0.02% w/v 200 31 44                                              300 61 45                                                                     Formulation C + 100 37 39                                                      Fluorad FC-135 0.05% w/v 200 49 43                                              300 66 62                                                                     Formulation C + 100 18 31                                                      Fluorad FC-135 0.02% w/v 200 47 44                                              300 68 49                                                                     Formulation C + 100 26 27                                                      Fluorad FC-135 0.01% w/v 200 36 44                                              300 54 82                                                                     Formulation C + 100 34 32                                                      Fluorad FC-754 0.05% w/v 200 47 37                                              300 62 62                                                                     Formulation C + 100 28 32                                                      Fluorad FC-754 0.02% w/v 200 45 60                                              300 43 75                                                                     31-01 100 16 36                                                                 200 54 56                                                                      300 66 61                                                                     31-02 100 23 43                                                                 200 45 45                                                                      300 65 51                                                                     31-03 100 31 35                                                                 200 37 45                                                                      300 53 60                                                                     31-04 100 24 35                                                                 200 43 43                                                                      300 78 50                                                                     31-05 100 24 36                                                                 200 45 44                                                                      300 58 66                                                                     31-06 100 31 24                                                                 200 46 34                                                                      300 52 51                                                                     31-07 100 49 33                                                                 200 65 39                                                                      300 73 63                                                                     31-08 100 48 25                                                                 200 70 49                                                                      300 73 69                                                                     31-09 100 45 27                                                                 200 59 53                                                                      300 71 84                                                                     31-10 100 60 30                                                                 200 64 89                                                                      300 75 99                                                                     31-11 100 47 51                                                                 200 66 65                                                                      300 80 78                                                                     31-12 100 49 39                                                                 200 60 59                                                                      300 67 84                                                                     31-13 100 50 30                                                                 200 70 51                                                                      300 68 66                                                                     31-14 100 54 33                                                                 200 61 44                                                                      300 79 66                                                                   ______________________________________                                    

In this test, glyphosate compositions containing egg yolk lecithin (31-01 to 31-03) performed similarly to those containing soybean lecithin (31-04 to 31-06) on ABUTH but were generally more effective than those containing soybean lecithin on ECHCF, at least in the absence of Fluorad FC-135. Addition of Fluorad FC-135, as in compositions 31-07 to 31-12, enhanced effectiveness of all compositions.

Example 32

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 32a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 32a                                                        ______________________________________                                         Spray      Lecithin                                                                               % w/w        Type of                                          composition g/l fluoro-organic fluoro-organic                                ______________________________________                                         32-01      0.20                 none                                             32-02 0.20 0.02 Fluorad FC-135                                                 32-03 0.20 0.02 Fluorad FC-431                                                 32-04 0.20 0.02 Fluorad FC-751                                                 32-05 0.20 0.02 Fluorad FC-170C                                                32-06 0.20 0.02 Fluorad FC-171                                                 32-07 0.20 0.02 Fluorad FC-754                                                 32-08 0.50  none                                                               32-09 0.10  none                                                               32-10 0.04  none                                                               32-11 0.02  none                                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and ECHCF, and 27 days after planting SIDSP. Evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 32-01 to 32-11, spray compositions were prepared by tank mixing Formulations B and C with various fluoro-organic surfactants of the Fluorad range, all at 0.02%. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 32b.

                  TABLE 32b                                                        ______________________________________                                                     Glyphosate                                                           rate % Inhibition                                                            Spray composition                                                                            g a.e./ha ABUTH    ECHCF SIDSP                                   ______________________________________                                         Formulation B 150        8       35    35                                         250 21 47 37                                                                   350 31 36 56                                                                   450 57 52 64                                                                  Formulation C 150 29 69 49                                                      250 55 90 67                                                                   350 75 91 75                                                                   450 82 91 85                                                                  Formulation B + 150 17 43 36                                                   Fluorad FC-135 0.02% w/v 250 39 58 53                                           350 52 53 68                                                                  Formulation B + 150 13 25 32                                                   Fluorad FC-170C 0.02% 250 31 47 36                                             w/v 350 31 85 61                                                               Formulation B + 150  8 52 15                                                   Fluorad FC-171 0.02% w/v 250 10 47 44                                           350 15 58 55                                                                  Formulation B + 150 14 36 34                                                   Fluorad FC-431 0.02% w/v 250 23 53 53                                           350 37 61 62                                                                  Formulation B + 150 12 29 29                                                   Fluorad FC-751 0.02% w/v 250 30 38 41                                           350 43 36 58                                                                  Formulation B + 150 21 27 33                                                   Fluorad FC-754 0.02% w/v 250 31 36 49                                           350 38 51 59                                                                  Formulation C + 150 35 31 46                                                   Fluorad FC-135 0.02% w/v 250 66 87 58                                           350 78 99 80                                                                  Formulation C + 150 29 68 41                                                   Fluorad FC-170C 0.02% 250 54 78 61                                             w/v 350 59 86 78                                                               Formulation C + 150 20 96 35                                                   Fluorad FC-171 0.02% w/v 250 37 99 62                                           350 55 100  65                                                                Formulation C + 150 20 94 41                                                   Fluorad FC-431 0.02% w/v 250 51 85 68                                           350 66 97 74                                                                  Formulation C + 150 15 67 38                                                   Fluorad FC-751 0.02% w/v 250 36 85 56                                           350 60 100  72                                                                Formulation C + 150 33 78 37                                                   Fluorad FC-754 0.02% w/v 250 75 85 66                                           350 82 94 80                                                                  32-01 150 25 35 45                                                              250 43 52 63                                                                   350 60 90 77                                                                  32-02 150 65 37 58                                                              250 69 69 67                                                                   350 66 69 78                                                                  32-03 150 14 40 41                                                              250 45 78 63                                                                   350 55 92 75                                                                  32-04 150 19 48 48                                                              250 36 51 63                                                                   350 65 69 70                                                                  32-05 150 47 34 45                                                              250 55 43 55                                                                   350 63 58 75                                                                  32-06 150 23 36 46                                                              250 57 52 59                                                                   350 61 73 67                                                                  32-07 150 67 59 58                                                              250 81 73 72                                                                   350 80 76 76                                                                  32-08 150 37 49 60                                                              250 60 83 69                                                                   350 67 93 49                                                                  32-09 150 19 63 51                                                              250 53 71 62                                                                   350 55 74 82                                                                  32-10 150 19 70 51                                                              250 39 94 61                                                                   350 63 87 73                                                                  32-11 150 16 51 50                                                              250 58 67 66                                                                   350 69 92 73                                                                ______________________________________                                    

Composition 32-07containing 0.02% lecithin and 0.02% Fluorad FC-754, was equal or superior to composition 32-02 containing 0.02% lecithin and 0.02% Fluorad FC-135, in herbicidal effectiveness. This indicates that Fluorad FC-754 is an acceptable substitute for Fluorad FC-135 in such compositions. The other fluoro-organic surfactants tested in this Example, none of which is cationic, were less effective than the cationic fluoro-organics Fluorad FC-135 and Fluorad FC-754 as excipients in combination with lecithin. A possible exception was Fluorad FC-170C which gave good enhancement of glyphosate effectiveness on ECHCF only.

Example 33

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 33a. Process (v) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 33a                                                        ______________________________________                                         % w/w                                                                            Concentrate                                                                              Glyphosate              Agrimul                                                                               Fluorad                               composition a.e. Lecithin MON 0818 PG-2069 FC-135                            ______________________________________                                         33-01   30        3.0             0.25   3.0                                     33-02 30 3.0  0.25 1.0                                                         33-03 30 3.0 0.25  3.0                                                         33-04 30 1.0 0.50  3.0                                                         33-05 30 1.0  0.50 3.0                                                         33-06 30 1.0   1.0                                                             33-07 30 1.0  0.25 1.0                                                         33-08 30 3.0  0.50 2.0                                                         33-09 30 2.0   3.0                                                             33-10 30 3.0 0.50                                                            ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and 17 days after planting ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 33b.

                  TABLE 33b                                                        ______________________________________                                                      Glyphosate rate                                                                          % Inhibition                                            Concentrate composition                                                                       g a.e./ha   ABUTH    ECHCF                                      ______________________________________                                         Formulation C   56          3        5                                            112 49 48                                                                      224 79 83                                                                      448 99 99                                                                     Formulation J  56 16 20                                                         112 40 43                                                                      224 80 81                                                                      448 97 99                                                                     33-01  56  4  5                                                                 112 35 20                                                                      224 81 51                                                                      448 99 80                                                                     33-02  56  0  5                                                                 112  4 20                                                                      224 66 55                                                                      448 94 80                                                                     33-03  56  1  5                                                                 112  6 20                                                                      224 78 74                                                                      448 93 80                                                                     33-04  56  1  5                                                                 112  1 15                                                                      224 75 65                                                                      448 95 80                                                                     33-05  56  0  5                                                                 112  1 15                                                                      224 75 65                                                                      448 91 80                                                                     33-06  56  0  5                                                                 112  3 15                                                                      224 55 63                                                                      448 91 79                                                                     33-07  56  1  5                                                                 112  3 15                                                                      224 48 55                                                                      448 88 81                                                                     33-08  56  3  9                                                                 112  3 20                                                                      224 66 60                                                                      448 89 80                                                                     33-09  56  0  5                                                                 112  5 10                                                                      224 78 55                                                                      448 97 80                                                                     33-10  56  0  5                                                                 112  4 15                                                                      224 21 55                                                                      448 88 79                                                                   ______________________________________                                    

Concentrate compositions containing lecithin and Fluorad FC-135 did not exhibit herbicidal effectiveness superior to commercial standard Formulations C and J in this test.

Example 34

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 34a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 34a                                                        ______________________________________                                         Spray         Lecithin                                                                               % w/w                                                      composition g/l Fluorad FC-135                                               ______________________________________                                         34-01         0.25                                                               34-02 0.05                                                                     34-03 0.02                                                                     34-04 0.01                                                                     34-05 0.25 0.25                                                                34-06 0.05 0.05                                                                34-07 0.02 0.02                                                                34-08 0.01 0.01                                                              ______________________________________                                    

Guineagrass (Panicum maximum, PANMA) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 78 days after planting PANMA, and evaluation of herbicidal inhibition was done 20 days after application.

In addition to compositions 34-01 to 34-08, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 34b.

                  TABLE 34b                                                        ______________________________________                                                          Glyphosate rate                                                                           % Inhibition                                         Spray composition g a.e./ha PANMA                                            ______________________________________                                         Formulation B    400        61                                                    800 89                                                                         1500 93                                                                        2000 97                                                                       Formulation C 400 85                                                            800 94                                                                         1500 100                                                                       2000 100                                                                      Formulation B + 400 76                                                         Fluorad FC-135 0.25% w/v 800 78                                                 1500 97                                                                       Formulation B + 400 45                                                         Fluorad FC-135 0.05% w/v 800 69                                                 1500 89                                                                       Formulation B + 400 39                                                         Fluorad FC-135 0.02% w/v 800 71                                                 1500 95                                                                       Formulation B + 400 52                                                         Fluorad FC-135 0.01% w/v 800 78                                                 1500 99                                                                       Formulation C + 400 82                                                         Fluorad FC-135 0.25% w/v 800 97                                                 1500 100                                                                      Formulation C + 400 63                                                         Fluorad FC-135 0.05% w/v 800 93                                                 1500 100                                                                      Formulation C + 400 73                                                         Fluorad FC-135 0.02% w/v 800 98                                                 1500 100                                                                      Formulation C + 400 66                                                         Fluorad FC-135 0.01% w/v 800 97                                                 1500 100                                                                      34-01 400 38                                                                    800 73                                                                         1500 92                                                                       34-02 400 64                                                                    800 83                                                                         1500 90                                                                       34-03 400 50                                                                    800 75                                                                         1500 99                                                                       34-04 400 48                                                                    800 88                                                                         1500 98                                                                       34-05 400 60                                                                    800 79                                                                         1500 99                                                                       34-06 400 58                                                                    800 86                                                                         1500 99                                                                       34-07 400 55                                                                    800 86                                                                         1500 93                                                                       34-08 400 60                                                                    800 91                                                                         1500 98                                                                     ______________________________________                                    

Exceptionally high glyphosate activity was seen in this test even with Formulation B and no firm conclusions can be drawn. However, none of the compositions containing lecithin and Fluorad FC-135 exceeded the effectiveness of commercial standard Formulation C on PANMA under the conditions of this test.

Example 35

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 35a. Process (v) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 35a                                                        ______________________________________                                         Concen-                                                                          trate % w/w                                                                  compo- Glyphosate        Fluorad                                                                              Fluorad                                                                              MON  Agrimul                                sition a.e. Lecithin FC-135 FC-754 0818 PG-2069                              ______________________________________                                         35-01  30        3.0     3.0              0.25                                   35-02 30 3.0 1.0   0.25                                                        35-03 30 3.0 3.0  0.25                                                         35-04 30 1.0 3.0  0.50                                                         35-05 30 1.0 3.0   0.50                                                        35-06 30 1.0 1.0                                                               35-07 30 1.0 1.0   0.25                                                        35-08 30 3.0 2.0   0.50                                                        35-09 30 2.0 3.0                                                               35-10 30 3.0   0.50                                                            35-11 30 3.0  3.0  0.50                                                        35-12 30 2.0  1.0   0.375                                                      35-13 30 1.0  2.0  0.25                                                        35-14 30 3.0  3.0 0.50                                                         35-15 30 3.0  3.0  0.50                                                        35-16 30 2.0  1.0   0.375                                                      35-17 30 1.0  2.0  0.25                                                        35-18 30 3.0  3.0 0.50                                                       ______________________________________                                    

Quackgrass (Elymus repens, AGRRE) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 56 days after planting AGRRE, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 35b.

                  TABLE 35b                                                        ______________________________________                                                         Glyphosate rate                                                                           % Inhibition                                          Concentrate composition g a.e./ha AGRRE                                      ______________________________________                                         Formulation B   400        41                                                     800 46                                                                         1000  55                                                                       1200  70                                                                      Formulation C 400 38                                                            800 47                                                                         1000  77                                                                       1200  77                                                                      Formulation J 400 60                                                            800 84                                                                         1000  77                                                                       1200  85                                                                      35-01 400 27                                                                    800 76                                                                         1000  79                                                                      35-02 400 49                                                                    800 66                                                                         1000  78                                                                      35-03 400 42                                                                    800 80                                                                         1000  83                                                                      35-04 400 31                                                                    800 71                                                                         1000  64                                                                      35-05 400 32                                                                    800 53                                                                         1000  59                                                                      35-06 400 27                                                                    800 39                                                                         1000  65                                                                      35-07 400 29                                                                    800 54                                                                         1000  61                                                                      35-08 400 38                                                                    800 65                                                                         1000  81                                                                      35-09 400 31                                                                    800 55                                                                         1000  67                                                                      35-10 400 43                                                                    800 38                                                                         1000  58                                                                      35-11 400 34                                                                    800 56                                                                         1000  75                                                                      35-12 400 29                                                                    800 51                                                                         1000  65                                                                      35-13 400 51                                                                    800 69                                                                         1000  83                                                                      35-14 400 39                                                                    800 63                                                                         1000  65                                                                      35-15 400 53                                                                    800 65                                                                         1000  77                                                                      35-16 400 43                                                                    800 65                                                                         1000  82                                                                      35-17 400 69                                                                    800 84                                                                         1000  94                                                                      35-18 400 69                                                                    800 92                                                                         1000  92                                                                    ______________________________________                                    

Compositions of the invention exhibiting superior herbicidal effectiveness to commercial standard Formulation C in this test on AGRRE included 35-01, 35-02, 35-03, 35-13 and 35-15 to 35-18. Compositions 35-17 and 35-18 were the most effective in this test, outperforming commercial standard Formulation J as well as Formulation C.

Example 36

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 36a. Process (v) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The order of addition of ingredients was varied in compositions 36-15 to 36-20 as shown below. The pH of all compositions was approximately 5.

                                      TABLE 36a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                               Fluorad                                                                            Agrimul                                                                             MON                                                                               Lecithin                                                                              order of                                        comp. a.e. Lecithin FC-135 PG-2069 0818 phospholipid % addition              __________________________________________________________________________                                      (*)                                           36-01                                                                              30    3.0 2.0 0.50    45     A                                               36-02 30 3.0 3.0 0.50  45 A                                                    36-03 30 3.0 3.0 0.75  45 A                                                    36-04 30 3.0 3.0 0.75 0.5 45 A(**)                                             36-05 30 3.0 3.0 1.00  45 A                                                    36-06 30 3.0 3.0 2.00  45 A                                                    36-07 30 3.0 3.0 3.00  45 A                                                    36-08 30 3.0 3.0 4.00  45 A                                                    36-09 30 3.0 2.0 0.50  20 A                                                    36-10 30 3.0 2.0 0.50  20 B                                                    36-11 30 3.0 2.0 0.50  20 C                                                    36-12 30 3.0 2.0 0.50  20 D                                                    36-13 30 3.0 2.0 0.50  20 E                                                    36-14 30 3.0 2.0 0.50  20 F                                                    36-15 30 3.0 3.0 0.50  20 A                                                    36-16 30 3.0 3.0 0.50  20 B                                                    36-17 30 3.0 3.0 0.50  20 C                                                    36-18 30 3.0 3.0 0.50  20 D                                                    36-19 30 3.0 3.0 0.50  20 E                                                    36-20 30 3.0 3.0 0.50  20 F                                                  __________________________________________________________________________

(*) Order of addition:

    ______________________________________                                         1st       2nd       3rd      4th     5th                                       ______________________________________                                         A   lecithin  PG-2069   FC-135 water   glyphosate                                B lecithin FC-135 PG-2069 water glyphosate                                     C glyphosate water FC-135 PG-2069 lecithin                                     D glyphosate water PG-2069 FC-135 lecithin                                     E glyphosate lecithin PG-2069 FC-135 water                                     F glyphosate lecithin FC-135 PG-2069 water                                   ______________________________________                                          (**) where MON 0818 included, added with Agrimul PG2069                  

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 22 days after planting ECHCF, and evaluation of herbicidal inhibition was done 17 days after application.

Formulations B, C and and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 33b.

                  TABLE 36b                                                        ______________________________________                                                    Glyphosate rate                                                                           % Inhibition                                             Concentrate composition                                                                     g a.e./ha    ABUTH    ECHCF                                       ______________________________________                                         Formulation B                                                                               200          38       73                                             400 51 64                                                                      600 67 89                                                                      800 72 86                                                                     Formulation C 200 57 75                                                         400 77 98                                                                      600 92 97                                                                      800 100   100                                                                 Formulation J 200 50 52                                                         400 73 99                                                                      600 88 99                                                                      800 98 98                                                                     36-01 200 49 64                                                                 400 72 59                                                                      600 78 87                                                                     36-02 200 54 72                                                                 400 78 71                                                                      600 97 90                                                                     36-03 200 57 62                                                                 400 80 78                                                                      600 89 87                                                                     36-04 200 46 39                                                                 400 74 64                                                                      600 86 78                                                                     36-05 200 49 29                                                                 400 74 79                                                                      600 83 90                                                                     36-06 200 49 65                                                                 400 70 88                                                                      600 87 88                                                                     36-07 200 49 51                                                                 400 67 77                                                                      600 81 83                                                                     36-08 200 42 59                                                                 400 70 67                                                                      600 78 80                                                                     36-09 200 45 28                                                                 400 73 85                                                                      600 87 98                                                                     36-10 200 57 82                                                                 400 76 89                                                                      600 87 98                                                                     36-11 200 56 80                                                                 400 84 84                                                                      600 85 100                                                                    36-12 200 57 81                                                                 400 78 98                                                                      600 87 94                                                                     36-13 200 54 86                                                                 400 73 72                                                                      600 96 97                                                                     36-14 200 56 73                                                                 400 69 98                                                                      600 85 94                                                                     36-15 200 40 41                                                                 400 85 88                                                                      600 83 96                                                                     36-16 200 53 59                                                                 400 73 76                                                                      600 84 73                                                                     36-17 200 39 53                                                                 400 65 86                                                                      600 86 81                                                                     36-18 200 49 31                                                                 400 69 52                                                                      600 73 75                                                                     36-19 200 47 50                                                                 400 74 86                                                                      600 88 98                                                                     36-20 200 51 42                                                                 400 68 94                                                                      600 90 98                                                                   ______________________________________                                    

Order of addition of ingredients apparently had some influence on herbicidal effectiveness of compositions 36-09 to 36-20. However, as most of these compositions showed poor short-term stability, it is likely that in at least some cases the uniformity of spray application was affected and the results are therefore difficult to interpret.

Example 37

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 37a. Process (iv) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 37a                                                        ______________________________________                                         Concen-                                                                          trate Glypho- % w/w                                                          compo-                                                                               sate            Aerosol                                                                              MON  Fluorad                                                                              Methyl                                    sition g a.e./l Lecithin OT 0818 FC-754 caprate PVA                          ______________________________________                                         37-01 200     2.0           0.25                                                 37-02 300 3.0  0.50                                                            37-03 300 3.0  0.50   2.0                                                      37-04 200 2.0  0.25   1.5                                                      37-05 200 2.0  0.25  1.0 1.0                                                   37-06 200 2.0  0.25  1.0 1.0                                                   37-07 200 2.0  0.25 2.0                                                        37-08 200  2.0 0.25                                                            37-09 300  3.0 0.50                                                            37-10 300  3.0 0.50   2.0                                                      37-11 200  2.0 0.25   1.5                                                      37-12 200  2.0 0.25  1.0                                                       37-13 200  2.0 0.25  1.0                                                       37-14 200  2.0 0.25  1.0 1.5                                                   37-15 200  2.0 0.25 2.0                                                      ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and 13 days after planting ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Compositions containing PVA were too viscous to spray and were not tested for herbicidal effectiveness. Formulations B, and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 37b.

                  TABLE 37b                                                        ______________________________________                                                    Glyphosate rate                                                                           % Inhibition                                             Concentrate composition                                                                     g a.e./ha    ABUTH    ECHCF                                       ______________________________________                                         Formulation B                                                                               112           5        4                                             224 48  8                                                                      336 73 20                                                                      448 94 50                                                                     Formulation C 112 30 45                                                         224 91 81                                                                      336 98 81                                                                      448 100  99                                                                   Formulation J 112 50 35                                                         224 80 65                                                                      336 97 88                                                                      448 100  90                                                                   37-01 112 11  8                                                                 224 50 40                                                                      336 71 61                                                                      448 93 78                                                                     37-02 112  5  6                                                                 224 64 58                                                                      336 78 60                                                                      448 84 65                                                                     37-07 112  5  3                                                                 224 46 38                                                                      336 73 83                                                                      448 93 66                                                                     37-08 112  8 13                                                                 224 43 46                                                                      336 73 65                                                                      448 83 70                                                                     37-09 112  1  5                                                                 224 23 25                                                                      336 65 33                                                                      448 91 58                                                                     37-12 112  0  5                                                                 224 58 48                                                                      336 73 63                                                                      448 91 63                                                                     37-13 112  0 10                                                                 224 53 38                                                                      336 73 45                                                                      448 88 50                                                                     37-15 112 28 10                                                                 224 50 53                                                                      336 80 63                                                                      448 88 91                                                                   ______________________________________                                    

Concentrate compositions containing lecithin and Fluorad FC-754 or methyl caprate did not exhibit herbicidal effectiveness equal to that of the commercial standards in this test.

Example 38

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 38a. Process (iii) was followed for all compositions, using soybean lecithin (20% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 38a                                                        ______________________________________                                                  % w/w                                                                 Concentrate                                                                               Glyphosate          Fluorad                                                                              MON                                         composition a.e. Lecithin FC-135 0818                                        ______________________________________                                         38-01      30        3.0       3.0   0.75                                        38-02 25 2.5 2.5 0.63                                                          38-03 20 2.0 2.0 0.50                                                          38-04 15 1.5 1.5 0.38                                                          38-05 10 1.0 1.0 0.25                                                          38-06  5 0.5 0.5 0.13                                                          38-07 30 3.0 3.0 1.50                                                          38-08 25 2.5 2.5 0.63                                                          38-09 20 2.0 2.0 0.50                                                          38-10 15 1.5 1.5 0.38                                                          38-11 10 1.0 1.0 0.25                                                          38-12  5 0.5 0.5 0.13                                                          38-13 25 2.5 2.5 0.94                                                          38-14 20 2.0 2.0 0.75                                                          38-15 15 1.5 1.5 0.56                                                          38-16 10 1.0 1.0 0.38                                                          38-17  5 0.5 0.5 0.19                                                        ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 14 days after application.

In addition to compositions 38-01 to 38-17, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at two concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 38b.

                  TABLE 38b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation C 200         59        98                                            400 96 96                                                                      600 70 93                                                                      800 100   97                                                                  Formulation C + 200 59 92                                                      Fluorad FC-135 0.1% 400 93 93                                                   600 95 100                                                                     800 100  97                                                                   Formulation C + 200 54 73                                                      Fluorad FC-135 0.05% 400 95 76                                                  600 100  82                                                                    800 100  95                                                                   Formulation J 200 55 87                                                         400 92 98                                                                      600 97 94                                                                      800 99 96                                                                     Formulation J + 200 67 88                                                      Fluorad FC-135 0.1% 400 89 89                                                   600 94 87                                                                      800 96 91                                                                     Formulation J + 200 71 81                                                      Fluorad FC-135 0.05% 400 75 95                                                  600 96 99                                                                      800 100  100                                                                  38-01 200 53 71                                                                 400 74 87                                                                      600 98 87                                                                     38-02 200 51 70                                                                 400 88 96                                                                      600 89 99                                                                     38-03 200 51 85                                                                 400 81 97                                                                      600 96 94                                                                     38-04 200 51 63                                                                 400 81 82                                                                      600 96 97                                                                     38-05 200 47 60                                                                 400 73 91                                                                      600 94 94                                                                     38-06 200 54 43                                                                 400 73 88                                                                      600 92 87                                                                     38-07 200 60 70                                                                 400 84 93                                                                      600 90 98                                                                     38-08 200 49 55                                                                 400 76 92                                                                      600 88 83                                                                     38-09 200 57 53                                                                 400 79 95                                                                      600 91 87                                                                     38-10 200 55 85                                                                 400 90 97                                                                      600 94 96                                                                     38-11 200 64 43                                                                 400 77 87                                                                      600 93 96                                                                     38-12 200 54 72                                                                 400 85 98                                                                      600 96 100                                                                    38-13 200 61 61                                                                 400 84 90                                                                      600 95 99                                                                     38-14 200 57 86                                                                 400 82 90                                                                      600 99 98                                                                     38-15 200 59 89                                                                 400 78 96                                                                      600 93 97                                                                     38-16 200 53 87                                                                 400 81 98                                                                      600 96 98                                                                     38-17 200 48 87                                                                 400 81 100                                                                     600 91 100                                                                  ______________________________________                                    

As concentrate compositions in previous Examples have tended to exhibit weaker herbicidal effectiveness than has been seen with ready-made spray compositions, this test was conducted to determine if the degree of concentration at which a composition is prepared before dilution for spraying had an influence on effectiveness. No consistent trend was seen in this test.

Example 39

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 39a. Process (iii) was followed for all compositions, using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 39a                                                        ______________________________________                                         % w/w                                                                                                  Fluorad                                                  Conc. Glyphosate  FC-135 or Amine Type of                                      comp. a.e. Lecithin FC-754 surfactant amine surfactant                       ______________________________________                                         39-01 20        2.0           0.25   MON 0818                                    39-02 20 3.0  0.25 MON 0818                                                    39-03 20 3.0 3.0 0.25 MON 0818                                                    (135)                                                                       39-04 20 3.0 3.0 0.25 MON 0818                                                    (754)                                                                       39-05 20 2.0  2.00 Triton RW-20                                                39-06 20 2.0  2.00 Triton RW-50                                                39-07 20 2.0  2.00 Triton RW-75                                                39-08 20 2.0  2.00 Triton RW-100                                               39-09 20 2.0  2.00 Triton RW-150                                               39-10 20   2.00 Triton RW-20                                                   39-11 20   2.00 Triton RW-50                                                   39-12 20   2.00 Triton RW-75                                                   39-13 20   2.00 Triton RW-100                                                  39-14 20   2.00 Triton RW-150                                                ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and 17 days after planting ECHCF, and evaluation of herbicidal inhibition was done 21 days after application.

Formulation C was applied as a comparative treatment. Results, averaged for all replicates of each treatment, are shown in Table 39b.

                  TABLE 39b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation C 112          0        10                                            224 10 20                                                                      336 47 30                                                                      448 63 40                                                                     39-01 112  8 15                                                                 224 25 35                                                                      336 55 56                                                                      448 63 65                                                                     39-02 112  5 10                                                                 224 23 33                                                                      336 55 64                                                                      448 66 60                                                                     39-03 112 28 15                                                                 224 55 35                                                                      336 74 58                                                                      448 76 65                                                                     39-04 112 15  8                                                                 224 53 45                                                                      336 73 55                                                                      448 75 64                                                                     39-05 112  0  8                                                                 224 14 45                                                                      336 45 70                                                                      448 65 66                                                                     39-06 112  1 13                                                                 224  5 43                                                                      336 58 64                                                                      448 66 75                                                                     39-07 112  0 15                                                                 224  1 53                                                                      336 45 78                                                                      448 60 83                                                                     39-08 112  0 10                                                                 224 25 45                                                                      336 50 79                                                                      448 68 88                                                                     39-09 112  0 13                                                                 224 13 45                                                                      336 50 75                                                                      448 70 81                                                                     39-10 112  0 18                                                                 224 18 35                                                                      336 48 65                                                                      448 66 76                                                                     39-11 112  1  0                                                                 224 35 25                                                                      336 38 55                                                                      448 50 78                                                                     39-12 112  8 25                                                                 224 10 38                                                                      336 48 70                                                                      448 73 81                                                                     39-13 112  0 25                                                                 224  5 33                                                                      336 30 70                                                                      448 74 75                                                                     39-14 112  0 12                                                                 224  0 30                                                                      336 12 70                                                                      448 40 80                                                                   ______________________________________                                    

No difference in herbicidal effectiveness was seen between compositions 39-03 and 39-04. The only difference between these compositions is that 39-03 contained Fluorad FC-135 and 39-04 contained Fluorad FC-754.

Example 40

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 40a. Process (iii) was followed for all compositions, using soybean lecithin (20% or 45% phospholipid as indicated below, both sourced from Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 40a                                                        ______________________________________                                                             % w/w                                                      Spray      Lecithin                                                                               Lecithin   Fluorad                                                                              Fluorad                                      composition g/l % purity FC-135 FC-754                                       ______________________________________                                         40-01      1.0     20                                                            40-02 0.5 20                                                                   40-03 0.2 20                                                                   40-04 1.0 20 0.10                                                              40-05 0.5 20 0.05                                                              40-06 0.2 20 0.02                                                              40-07 1.0 20  0.10                                                             40-08 0.5 20  0.05                                                             40-09 0.2 20 0.02 0.02                                                         40-10 0.5 45 0.05                                                              40-11 0.5 45  0.05                                                           ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

In addition to compositions 40-01 to 40-11, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 or FC-754 at various concentrations. Formulations B and C alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 40b.

                  TABLE 40b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Spray composition                                                                            g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         49        100                                           300 66 92                                                                      500 80 76                                                                      700 93 96                                                                     Formulation C 200 57 79                                                         400 93 98                                                                      600 100  100                                                                   800 100  100                                                                  Formulation B + 200 58 80                                                      Fluorad FC-135 0.1% 400 63 100                                                  600 82 100                                                                    Formulation B + 200 37 49                                                      Fluorad FC-135 0.05% 400 67 84                                                  600 74 100                                                                    Formulation B + 200 33 82                                                      Fluorad FC-135 0.02% 400 58 94                                                  600 81 87                                                                     Formulation B + 200 50 45                                                      Fluorad FC-754 0.1% 400 77 82                                                   600 77 94                                                                     Formulation B + 200 44 45                                                      Fluorad FC-754 0.05% 400 71 65                                                  600 74 90                                                                     Formulation B + 200 31 57                                                      Fluorad FC-754 0.02% 400 67 83                                                  600 68 93                                                                     Formulation C + 200 69 65                                                      Fluorad FC-135 0.1% 400 91 99                                                   600 97 100                                                                    Formulation C + 200 73 87                                                      Fluorad FC-135 0.05% 400 89 100                                                 600 98 100                                                                    Formulation C + 200 51 60                                                      Fluorad FC-135 0.02% 400 91 100                                                 600 98 100                                                                    Formulation C + 200 70 81                                                      Fluorad FC-754 0.1% 400 85 99                                                   600 98 95                                                                     Formulation C + 200 68 54                                                      Fluorad FC-754 0.05% 400 78 88                                                  600 91 88                                                                     Formulation C + 200 50 41                                                      Fluorad FC-754 0.02% 400 89 91                                                  600 99 100                                                                    40-01 200 41 37                                                                 400 78 84                                                                      600 83 100                                                                    40-02 200 38 82                                                                 400 74 94                                                                      600 82 98                                                                     40-03 200 38 62                                                                 400 69 85                                                                      600 86 100                                                                    40-04 200 63 69                                                                 400 79 75                                                                      600 93 89                                                                     40-05 200 69 66                                                                 400 85 81                                                                      600 84 86                                                                     40-06 200 64 38                                                                 400 79 74                                                                      600 93 99                                                                     40-07 200 61 43                                                                 400 76 71                                                                      600 85 85                                                                     40-08 200 71 52                                                                 400 82 85                                                                      600 82 100                                                                    40-09 200 63 55                                                                 400 83 73                                                                      600 79 97                                                                     40-10 200 65 54                                                                 400 78 80                                                                      600 85 99                                                                     40-11 200 55 33                                                                 400 77 74                                                                      600 91 97                                                                   ______________________________________                                    

There was a tendency, although not consistently so, for compositions of this Example containing Fluorad FC-754 to show slightly weaker herbicidal effectiveness than corresponding compositions containing Fluorad FC-135.

Example 41

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 41a. Process (v) was followed for all compositions, using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 41a                                                        ______________________________________                                         % w/w                                                                            Concentrate                                                                              Glyphosate      Fluorad                                                                              Fluorad                                        composition a.e. Lecithin FC-135 FC-754 MON 0818                             ______________________________________                                         41-01   15.0      4.0     8.0         0.5                                        41-02 15.0 6.0 8.0  0.5                                                        41-03 15.0 8.0 8.0  0.5                                                        41-04 10.0 4.0 8.0  0.5                                                        41-05 10.0 6.0 8.0  0.5                                                        41-06 10.0 8.0 8.0  0.5                                                        41-07 5.0 4.0 8.0  0.5                                                         41-08 5.0 6.0 8.0  0.5                                                         41-09 5.0 8.0 8.0  0.5                                                         41-10 15.0 4.0  8.0 0.5                                                        41-11 15.0 6.0  8.0 0.5                                                        41-12 15.0 8.0  8.0 0.5                                                        41-13 10.0 4.0  8.0 0.5                                                        41-14 10.0 6.0  8.0 0.5                                                        41-15 10.0 8.0  8.0 0.5                                                        41-16 5.0 4.0  8.0 0.5                                                         41-17 5.0 6.0  8.0 0.5                                                         41-18 5.0 8.0  8.0 0.5                                                       ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 20 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 41-01 to 41-18, spray compositions were prepared by tank mixing Formulations B and J with Fluorad FC-135 at two concentrations. Formulations B and J alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 41b.

                  TABLE 41b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         49        41                                            300 41 55                                                                      500 76 98                                                                      700 82 100                                                                    Formulation J 150 59 66                                                         300 79 99                                                                      500 93 99                                                                      700 98 100                                                                    Formulation B + 150 52 85                                                      Fluorad FC-135 0.1% 300 69 93                                                   500 89 97                                                                     Formulation B + 150  9 61                                                      Fluorad FC-135 0.05% 300 71 77                                                  500 77 100                                                                    Formulation J + 150 52 99                                                      Fluorad FC-135 0.1% 300 74 100                                                  500 82 99                                                                     Formulation J + 150 41 52                                                      Fluorad FC-135 0.05% 300 77 83                                                  500 91 100                                                                    41-01 150 66 51                                                                 300 86 91                                                                      500 93 100                                                                    41-02 150 72 88                                                                 300 89 93                                                                      500 96 92                                                                     41-03 150 71 91                                                                 300 89 95                                                                      500 91 100                                                                    41-04 150 63 90                                                                 300 89 89                                                                      500 96 99                                                                     41-05 150 70 79                                                                 300 84 94                                                                      500 88 98                                                                     41-06 150 69 76                                                                 300 89 84                                                                      500 94 100                                                                    41-07 150 71 87                                                                 300 77 82                                                                      500 99 92                                                                     41-08 150 81 87                                                                 300 88 94                                                                      500 92 98                                                                     41-09 150 72 83                                                                 300 87 83                                                                      500 94 94                                                                     41-10 150 72 70                                                                 300 81 80                                                                      500 89 93                                                                     41-11 150 74 85                                                                 300 87 96                                                                      500 91 98                                                                     41-12 150 66 92                                                                 300 78 98                                                                      500 93 100                                                                    41-13 150 71 76                                                                 300 86 95                                                                      500 94 99                                                                     41-14 150 72 75                                                                 300 90 97                                                                      500 91 99                                                                     41-15 150 69 82                                                                 300 85 98                                                                      500 94 100                                                                    41-16 150 76 87                                                                 300 86 100                                                                     500 90 99                                                                     41-17 150 71 83                                                                 300 87 94                                                                      500 96 100                                                                    41-18 150 70 81                                                                 300 77 98                                                                      500 89 98                                                                   ______________________________________                                    

Good herbicidal effectiveness was obtained with the concentrate compositions of this Example containing lecithin and Fluorad FC-135 or Fluorad FC-754. No great or consistent difference was seen between compositions containing Fluorad FC-135 and their counterparts containing Fluorad FC-754.

Example 42

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 42a. Process (v) was followed for all compositions, using soybean lecithin (95% phospholipid, Avanti). The pH of all compositions was approximately 5.

                                      TABLE 42a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                               MON Agrimul                                                                             Fluorad                                                                            Fluorad                                                                            Westvaco                                          comp. a.e. Lecithin 0818 PG-2069 FC-135 FC-754 H-240                         __________________________________________________________________________     42-01                                                                              30    3.0     0.25 3.0     9.0                                               42-02 30 3.0  0.25 1.0  9.0                                                    42-03 30 3.0 0.25  3.0  9.0                                                    42-04 30 1.0 0.50  3.0  9.0                                                    42-05 30 1.0  0.50 3.0  9.0                                                    42-06 30 1.0   1.0  9.0                                                        42-07 30 1.0  0.25 1.0  9.0                                                    42-08 30 3.0  0.50 2.0  9.0                                                    42-09 30 2.0   3.0  9.0                                                        42-10 30 3.0     5.0                                                           42-11 30 3.0  0.50  3.0 9.0                                                    42-12 30 2.0  0.38  2.0 9.0                                                    42-13 30 1.0  0.25  1.0 9.0                                                    42-14 30 3.0 0.50   3.0 9.0                                                    42-15 15 6.0 2.00  8.3                                                         42-16 15 6.0 4.00  8.3                                                       __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and 20 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 42-01 to 42-16, spray compositions were prepared by tank mixing Formulations B and J with Fluorad FC-135 at two concentrations. Formulations B and J alone were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 42b.

                  TABLE 42b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          3        33                                            300 12 90                                                                      500 65 98                                                                      700 79 100                                                                    Formulation J 150  2 46                                                         300 76 100                                                                     500 98 100                                                                     700 98 100                                                                    Formulation B + 150 10 38                                                      Fluorad FC-135 0.1% 300 50 85                                                   500 65 68                                                                     Formulation B + 150  3 27                                                      Fluorad FC-135 0.05% 300 36 82                                                  500 68 99                                                                     Formulation J + 150 18 79                                                      Fluorad FC-135 0.1% 300 57 98                                                   500 79 100                                                                    Formulation J + 150  2 37                                                      Fluorad FC-135 0.05% 300 56 97                                                  500 96 98                                                                     42-01 150  2 27                                                                 300  2 74                                                                      500 46 78                                                                     42-02 150  2 52                                                                 300 41 64                                                                      500 40 85                                                                     42-03 150  3 38                                                                 300 39 47                                                                      500 73 98                                                                     42-04 150  3 38                                                                 300 42 63                                                                      500 78 84                                                                     42-05 150  5 29                                                                 300 37 89                                                                      500 70 99                                                                     42-06 150  8 37                                                                 300 30 89                                                                      500 69 97                                                                     42-07 150  5 53                                                                 300 32 80                                                                      500 83 99                                                                     42-08 150  3 26                                                                 300 10 40                                                                      500 12 55                                                                     42-09 150  7 21                                                                 300 57 86                                                                      500 91 97                                                                     42-10 150 21 61                                                                 300 73 89                                                                      500 85 98                                                                     42-11 150  6 23                                                                 300 53 70                                                                      500 85 83                                                                     42-12 150 33 25                                                                 300 34 43                                                                      500 83 97                                                                     42-13 150  7 34                                                                 300 62 39                                                                      500 77 73                                                                     42-14 150 10 27                                                                 300 59 40                                                                      500 84 73                                                                     42-15 150 71 48                                                                 300 97 65                                                                      500 99 92                                                                     42-16 150 83 40                                                                 300 98 89                                                                      500 100  95                                                                 ______________________________________                                    

The only concentrate compositions in this test exhibiting excellent performance, at least on ABUTH, were 42-15 and 42-16.

Example 43

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 43a. Process (viii) was followed for composition 43-02 and process (ix) for compositions 43-03 to 43-13 which contain a colloidal particulate together with surfactant. Composition 43-01 contains colloidal particulate but no surfactant. The pH of all compositions was approximately 5.

                  TABLE 43a                                                        ______________________________________                                                % w/w                                                                   Concentrate                                                                             Glyphosate Fluorad           Emphos                                     composition a.e. FC-135 Aerosil 90 PS-21A                                    ______________________________________                                         43-01    20                  3.3                                                 43-02 20 3.3                                                                   43-03 31 1.1 3.3 1.1                                                           43-04 31 1.1 3.3 2.2                                                           43-05 31 1.1 3.3 3.3                                                           43-06 31 2.2 3.3 1.1                                                           43-07 31 2.2 3.3 2.2                                                           43-08 31 2.2 3.3 3.3                                                           43-09 31 3.3 3.3 1.1                                                           43-10 31 3.3 3.3 2.2                                                           43-11 31 3.3 3.3 3.3                                                           43-12 31 3.3 3.3                                                               43-13 31  3.3 3.3                                                            ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and 17 days after planting ECHCF, and evaluation of herbicidal inhibition was done 23 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 43b.

                  TABLE 43b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0         8                                            250 18 25                                                                      350 35 40                                                                      450 75 50                                                                     Formulation C 150 30 85                                                         250 92 95                                                                      350 100  100                                                                   450 100  100                                                                  Formulation J 150 40 70                                                         250 70 83                                                                      350 93 92                                                                      450 100  98                                                                   43-01 150 20 25                                                                 250 35 30                                                                      350 65 43                                                                      450 73 35                                                                     43-02 150  5  5                                                                 250 20 25                                                                      350 45 35                                                                      450 66 83                                                                     43-03 150 20 11                                                                 250 40 30                                                                      350 73 64                                                                      450 88 83                                                                     43-04 150 15  3                                                                 250 30 25                                                                      350 40 35                                                                      450 71 75                                                                     43-05 150 15 10                                                                 250 33 30                                                                      350 69 45                                                                      450 78 65                                                                     43-06 150 11  8                                                                 250 28 30                                                                      350 30 35                                                                      450 69 61                                                                     43-07 150  5  8                                                                 250 13 20                                                                      350 51 30                                                                      450 74 43                                                                     43-08 150 15  8                                                                 250 30 15                                                                      350 35 30                                                                      450 56 45                                                                     43-09 150 15 15                                                                 250 28 20                                                                      350 43 33                                                                      450 45 40                                                                     43-10 150  5  3                                                                 250 25 20                                                                      350 50 40                                                                      450 48 58                                                                     43-11 150 14  6                                                                 250 25 40                                                                      350 64 76                                                                      450 78 79                                                                     43-12 150  9 20                                                                 250 20 33                                                                      350 46 73                                                                      450 59 80                                                                     43-13 150 15 11                                                                 250 20 28                                                                      350 30 59                                                                      450 68 48                                                                   ______________________________________                                    

Most concentrate compositions containing Fluorad FC-135 showed enhanced herbicidal effectiveness by comparison with Formulation B but did not equal the performance of commercial standard Formulations C and J under the conditions of this test.

Example 44

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 44a. Process (viii) was followed for compositions 44-01, 44-03, 44-06, 44-07, 44-10, 44-14, 44-15, 44-18 and 44-19 process (ix) for compositions 44-02, 44-08, 44-09, 44-16 and 44-17 which contain a colloidal particulate together with surfactant. Compositions 44-04, 44-05, 44-12 and 44-13 contain colloidal particulate but no surfactant. The pH of all compositions was approximately 5.

                                      TABLE 44a                                    __________________________________________________________________________     % w/w                                                                          Concentrate                                                                          Glyphosate                                                                           Fluorad                                                                            Ethomeen                                                                            Aluminum                                                                            Titanium                                               composition a.e. FC-135 T/25 oxide C dioxide P25 Aerosol OT                  __________________________________________________________________________     44-01 20        3.30                                                             44-02 20     3.30                                                              44-03 20 3.30                                                                  44-04 20   3.30                                                                44-05 20   0.67                                                                44-06 20  3.30 3.30                                                            44-07 20  3.30 0.67                                                            44-08 20   3.30  3.30                                                          44-09 20   0.67  3.30                                                          44-10 20 3.30  3.30                                                            44-11 20 3.30  0.67                                                            44-12 20    3.30                                                               44-13 20    0.67                                                               44-14 20  3.30  3.30                                                           44-15 20  3.30  0.67                                                           44-16 20    3.30 3.30                                                          44-17 20    0.67 3.30                                                          44-18 20 3.30   3.30                                                           44-19 20 3.30   0.67                                                         __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 20 days after planting ECHCF, and evaluation of herbicidal inhibition was done 25 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 44b.

                  TABLE 44b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          8        45                                            250 37 55                                                                      350 40 60                                                                      450 50 70                                                                     Formulation C 150 27 72                                                         250 73 92                                                                      350 90 99                                                                      450 92 99                                                                     Formulation J 150 25 66                                                         250 45 88                                                                      350 78 99                                                                      450 91 100                                                                    44-01 150 40 82                                                                 250 55 93                                                                      350 74 100                                                                     450 83 100                                                                    44-02 150  9 20                                                                 250 30 73                                                                      350 38 73                                                                      450 55 97                                                                     44-03 150 13 23                                                                 250 35 79                                                                      350 45 78                                                                      450 75 100                                                                    44-04 150 18 45                                                                 250 35 65                                                                      350 35 70                                                                      450 68 81                                                                     44-05 150 11 43                                                                 250 35 50                                                                      350 50 55                                                                      450 59 78                                                                     44-06 150 25 75                                                                 250 58 93                                                                      350 88 100                                                                     450 95 100                                                                    44-07 150 15 88                                                                 250 68 100                                                                     350 79 100                                                                     450 90 100                                                                    44-08 150 28 38                                                                 250 25 38                                                                      350 35 55                                                                      450 71 79                                                                     44-09 112  5 13                                                                 224 23 48                                                                      336 25 70                                                                      448 45 64                                                                     44-10 150  1 20                                                                 250 40 74                                                                      350 65 55                                                                      450 84 96                                                                     44-11 150 25 25                                                                 250 35 65                                                                      350 45 61                                                                      450 76 92                                                                     44-12 150 14 28                                                                 250 40 43                                                                      350 45 70                                                                      450 65 79                                                                     44-13 150 20 45                                                                 250 48 33                                                                      350 60 55                                                                      450 80 79                                                                     44-14 150 23 79                                                                 250 73 100                                                                     350 76 99                                                                      450 85 99                                                                     44-15 150 25 83                                                                 250 69 99                                                                      350 75 99                                                                      450 91 100                                                                    44-16 150 14 28                                                                 250 23 40                                                                      350 30 79                                                                      450 69 86                                                                     44-17 150  1 20                                                                 250 23 33                                                                      350 16 45                                                                      450 40 68                                                                     44-18 150  8 15                                                                 250 49 56                                                                      350 55 58                                                                      450 83 83                                                                     44-19 150  6 15                                                                 250 35 60                                                                      350 61 63                                                                      450 63 70                                                                   ______________________________________                                    

Concentrate compositions containing Fluorad FC-135 showed enhanced herbicidal effectiveness by comparison with Formulation B but did not provide herbicidal effectiveness equal to commercial standard Formulations C and J in this test.

Example 45

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 45a. Process (i) was followed for compositions 45-10 to 45-12 and process (iii) for compositions 45-01 to 45-09 using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 45a                                                        ______________________________________                                         Spray     % w/w                                                                composition                                                                              Lecithin   Fluorad FC-135                                                                             Surf H1                                       ______________________________________                                         45-01     0.10                                                                   45-02 0.05                                                                     45-03 0.02                                                                     45-04 0.10 0.10                                                                45-05 0.05 0.05                                                                45-06 0.02 0.02                                                                45-07 0.10  0.10                                                               45-08 0.05  0.05                                                               45-09 0.02  0.02                                                               45-10   0.10                                                                   45-11   0.05                                                                   45-12   0.02                                                                 ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 23 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

In addition to compositions 45-01 to 45-12, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone and Formulation J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 45b.

                  TABLE 45b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Spray composition                                                                            g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         16        21                                            250 68 32                                                                      350 68 63                                                                      450 67 69                                                                     Formulation C 150 29 47                                                         250 76 74                                                                      350 98 94                                                                      450 100   85                                                                  Formulation J 150 37 31                                                         250 79 72                                                                      350 93 82                                                                      450 97 97                                                                     Formulation B + 150 55 15                                                      Fluorad FC-135 0.1% w/v 250 73 28                                               350 85 57                                                                      450 83 83                                                                     Formulation B + 150 59 15                                                      Fluorad FC-135 0.05% w/v 250 77 41                                              350 81 72                                                                      450 77 51                                                                     Formulation B + 150 25 12                                                      Fluorad FC-135 0.02% w/v 250 54 27                                              350 82 38                                                                      450 75 47                                                                     Formulation C + 150 51 26                                                      Fluorad FC-135 0.1% w/v 250 78 63                                               350 86 71                                                                      450 89 79                                                                     Formulation C + 150 58 23                                                      Fluorad FC-135 0.05% w/v 250 74 89                                              350 93 78                                                                      450 89 91                                                                     45-01 150 29 26                                                                 250 61 47                                                                      350 73 48                                                                      450 82 62                                                                     45-02 150 34 34                                                                 250 67 34                                                                      350 73 54                                                                      450 85 43                                                                     45-03 150 20 29                                                                 250 60 49                                                                      350 68 84                                                                      450 74 64                                                                     45-04 150 78 24                                                                 250 83 33                                                                      350 96 64                                                                      450 97 59                                                                     45-05 150 81 21                                                                 250 89 27                                                                      350 82 34                                                                      450 99 31                                                                     45-06 150 92 14                                                                 250 85 64                                                                      350 86 31                                                                      450 90 60                                                                     45-07 150 71 27                                                                 250 81 46                                                                      350 84 66                                                                      450 88 62                                                                     45-08 150 46 29                                                                 250 70 43                                                                      350 78 61                                                                      450 86 58                                                                     45-09 150 55 25                                                                 250 76 33                                                                      350 80 50                                                                      450 78 62                                                                     45-10 150 65 26                                                                 250 85 28                                                                      350 91 37                                                                      450 89 53                                                                     45-11 150 73 27                                                                 250 77 28                                                                      350 92 41                                                                      450 92 49                                                                     45-12 150 71 20                                                                 250 74 31                                                                      350 79 39                                                                      450 93 53                                                                   ______________________________________                                    

Extremely high herbicidal effectiveness was noted on ABUTH with compositions 45-04 to 45-06, containing lecithin and Fluorad FC-135. Replacement of Fluorad FC-135 by "Surf H1", a hydrocarbon-base surfactant of formula C₁₂ H₂₅ SO₂ NH(CH₂)₃ N⁺ (CH₃)₃ I⁻, gave (in compositions 45-07 to 45-09) effectiveness on ABUTH still superior at low glyphosate rates to commercial standard Formulations C and J were not quite as great as that of compositions 45-04 to 45-06. Performance of compositions 45-04 to 45-12 on ECHCF was relatively low in this test but performance on ABUTH was remarkably high considering the very low surfactant concentrations present.

Example 46

Aqueous spray compositions were prepared containing glyphosate IPA or tetrabutylammonuium salt and excipient ingredients as shown in Table 46a. Process (i) was followed for compositions 46-10 to 46-13 and process (iii) for compositions 46-01 to 46-09 using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was adjusted to approximately 7.

                  TABLE 46a                                                        ______________________________________                                         % w/w                                                                          Spray                    Fluorad      Glyphosate                                 composition Lecithin LI-700 FC-135 Surf H1 salt                              ______________________________________                                         46-01   0.10                          IPA                                        46-02 0.05    IPA                                                              46-03 0.02    IPA                                                              46-04 0.10  0.10  IPA                                                          46-05 0.05  0.05  IPA                                                          46-06 0.02  0.02  IPA                                                          46-07 0.10   0.10 IPA                                                          46-08 0.05   0.05 IPA                                                          46-09 0.02   0.02 IPA                                                          46-10  0.10   IPA                                                              46-11  0.05   IPA                                                              46-12  0.02   IPA                                                              46-13     (BU).sub.4 N                                                         46-14 0.05  0.05  (BU).sub.4 N                                                 46-15   0.05  (BU).sub.4 N                                                   ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 21 days after planting ECHCF, and evaluation of herbicidal inhibition was done 14 days after application.

In addition to compositions 46-01 to 46-15, spray compositions were prepared by tank mixing Formulations B and C with Fluorad FC-135 at various concentrations. Formulations B and C alone and Formulation J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 46b.

                  TABLE 46b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Spray composition                                                                            g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         33        24                                            300 51 27                                                                      500 68 36                                                                      700 83 43                                                                     Formulation C 150 32 30                                                         300 78 68                                                                      500 90 81                                                                      700 96 89                                                                     Formulation J 150 16 27                                                         300 74 56                                                                      500 88 79                                                                      700 93 92                                                                     Formulation B +  150 22 18                                                     Fluorad FC-135 0.1% w/v 300 71 26                                               500 73 51                                                                     Formulation B + 150 19 16                                                      Fluorad FC-135 0.05% w/v 300 60 28                                              500 72 33                                                                     Formulation B + 150 14 14                                                      Fluorad FC-135 0.02% w/v 300 23 26                                              500 69 38                                                                     Formulation C + 150 31 11                                                      Fluorad FC-135 0.1% w/v 300 73 27                                               500 82 48                                                                     Formulation C + 150 43 23                                                      Fluorad FC-135 0.05% w/v 300 71 49                                              500 93 50                                                                     46-01 150 20 18                                                                 300 65 29                                                                      500 85 34                                                                     46-02 150 22 19                                                                 300 63 35                                                                      500 83 51                                                                     46-03 150 24 29                                                                 300 64 35                                                                      500 85 40                                                                     46-04 150 63 21                                                                 300 75 31                                                                      500 84 46                                                                     46-05 150 68 10                                                                 300 82 29                                                                      500 81 53                                                                     46-06 150 68 21                                                                 300 84 30                                                                      500 85 46                                                                     46-07 150 41 35                                                                 300 51 39                                                                      500 93 61                                                                     46-08 150 34 22                                                                 300 77 27                                                                      500 85 35                                                                     46-09 150 24 17                                                                 300 78 39                                                                      500 91 58                                                                     46-10 150 16 19                                                                 300 62 28                                                                      500 72 53                                                                     46-11 150 38 25                                                                 300 59 38                                                                      500 82 59                                                                     46-12 150  7 23                                                                 300 61 40                                                                      500 77 63                                                                     46-13 150 81 48                                                                 300 92 51                                                                      500 90 46                                                                     46-14 150 87 30                                                                 300 91 69                                                                      500 95 89                                                                     46-15 150 81 37                                                                 300 94 41                                                                      500 92 63                                                                   ______________________________________                                    

As in the previous Example, compositions containing "Surf H1" did not show as strong enhancement of glyphosate effectiveness as counterpart compositions containing Fluorad FC-135. The tetrabutylammonium salt of glyphosate (compositions 46-13 to 46-15) exhibited extremely high herbicidal effectiveness in this test.

Example 47

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 47a. Process (v) was followed for all compositions using soybean lecithin (45% phospholipid, Avanti), except that various orders of addition were tried as indicated below. The pH of all compositions was approximately 5.

                                      TABLE 47a                                    __________________________________________________________________________     % w/w                           Order of                                       Concentrate                                                                          Glyphosate                                                                               Fluorad                                                                            Fluorad                                                                            MON                                                                               Agrimul                                                                             addition                                         composition a.e. Lecithin FC-135 FC-754 0818 PG-2069 (*)                     __________________________________________________________________________     47-01 30    3.0 3.0     0.75    A                                                47-02 30 3.0 3.0  0.75  B                                                      47-03 30 3.0 3.0  0.75  C                                                      47-04 30 3.0 3.0  0.75  D                                                      47-05 30 3.0 3.0  0.75  E                                                      47-06 30 3.0 3.0  0.75  F                                                      47-07 30 3.0  3.0 0.75  A                                                      47-08 30 3.0  3.0 0.75  B                                                      47-09 30 3.0  3.0 0.75  C                                                      47-10 30 3.0  3.0 0.75  D                                                      47-11 30 3.0  3.0 0.75  E                                                      47-12 30 3.0  3.0 0.75  F                                                      47-13 30 3.0 3.0   0.5 A                                                       47-14 30 3.0 3.0   0.5 B                                                       47-15 30 3.0 3.0   0.5 C                                                       47-16 30 3.0 3.0   0.5 D                                                       47-17 30 3.0 3.0   0.5 E                                                       47-18 30 3.0 3.0   0.5 F                                                     __________________________________________________________________________

(*) Order of addition:

    ______________________________________                                         1st      2nd      3rd        4th     5th                                       ______________________________________                                         A   lecithin MON/PG   FC-135/754                                                                              water   glyphosate                                B lecithin FC-135 MON/PG water glyphosate                                      C glyphosate water FC-135/754 MON/PG lecithin                                  D glyphosate water MON/PG FC-135/754 lecithin                                  E glyphosate lecithin MON/PG FC-135/754 water                                  F glyphosate lecithin FC-135/754 MON/PG water                                ______________________________________                                          MON/PG means MON 0818 or Agrimul PG2069                                  

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 15 days after planting ABUTH and 18 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 47b.

                  TABLE 47b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation C 150         26        69                                            300 75 100                                                                     500 85 99                                                                      700 94 100                                                                    Formulation J 150 38 78                                                         300 76 87                                                                      500 87 100                                                                     700 90 100                                                                    47-01 150 10 35                                                                 300 51 56                                                                      500 71 91                                                                      700 77 100                                                                    47-02 150 24 35                                                                 300 57 71                                                                      500 77 93                                                                      700 94 100                                                                    47-03 150 11 33                                                                 300 48 55                                                                      500 73 87                                                                      700 83 93                                                                     47-04 150 37 36                                                                 300 50 38                                                                      500 68 94                                                                     47-05 150 24 32                                                                 300 48 47                                                                      500 77 85                                                                      700 76 100                                                                    47-06 150 12 32                                                                 300 61 40                                                                      500 83 86                                                                      700 88 95                                                                     47-07 150 17 25                                                                 300 58 77                                                                      500 73 97                                                                      700 86 81                                                                     47-08 150 12 34                                                                 300 53 47                                                                      500 69 72                                                                      700 79 100                                                                    47-09 150 10 33                                                                 300 47 70                                                                      500 67 99                                                                      700 83 81                                                                     47-10 150 13 25                                                                 300 49 51                                                                      500 70 73                                                                      700 85 92                                                                     47-11 150 10 22                                                                 300 56 37                                                                      500 77 47                                                                      700 85 85                                                                     47-12 150 13 27                                                                 300 61 68                                                                      500 78 52                                                                      700 86 85                                                                     47-13 150 14 27                                                                 300 62 35                                                                      500 72 46                                                                      700 87 67                                                                     47-14 150 15 27                                                                 300 59 37                                                                      500 76 63                                                                      700 85 61                                                                     47-15 150 10 25                                                                 300 40 46                                                                      500 72 88                                                                      700 79 51                                                                     47-16 150 12 27                                                                 300 53 41                                                                      500 63 49                                                                      700 71 85                                                                     47-17 150 23 25                                                                 300 59 35                                                                      500 70 79                                                                      700 75 86                                                                     47-18 150 10 27                                                                 300 56 39                                                                      500 69 57                                                                      700 74 93                                                                   ______________________________________                                    

No great or consistent differences in herbicidal effectiveness were seen with different orders of addition of ingredients.

Example 48

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 48a. Process (v) was followed for all compositions using soybean lecithin (45% phospholipid, Avanti). Order of addition of ingredients was varied as indicated below. The pH of all compositions was approximately 5.

                  TABLE 48a                                                        ______________________________________                                         % w/w                                                                          Concentrate                                                                            Glyphosate        Fluorad                                                                              MON   Order of                                   composition a.e. Lecithin FC-135 0818 addition (*)                           ______________________________________                                         48-01   20        6.0     6.0   2.0   A                                          48-02 20 6.0 6.0 2.0 B                                                         48-03 20 6.0 6.0 2.0 C                                                         48-04 20 6.0 3.0 2.0 A                                                         48-05 20 6.0 3.0 2.0 B                                                         48-06 20 6.0 3.0 2.0 C                                                         48-07 20 6.0 1.0 2.0 A                                                         48-08 20 6.0 1.0 2.0 B                                                         48-09 20 6.0 1.0 2.0 C                                                         48-10 20 6.0 0.0 2.0 A                                                         48-11 20 6.0 0.0 2.0 B                                                         48-12 20 6.0 0.0 2.0 C                                                         48-13 20 2.0 2.0 0.5 A                                                         48-14 20 2.0 2.0 0.5 B                                                         48-15 20 2.0 2.0 0.5 C                                                       ______________________________________                                    

(*) Order of addition:

    ______________________________________                                         1st         2nd      3rd      4th   5th                                        ______________________________________                                         A    lecithin   MON      FC-135 water glyphosate                                   0818                                                                         B lecithin MON water FC-135 glyphosate                                           0818                                                                         C lecithin water MON FC-135 glyphosate                                            0818                                                                      ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and 16 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 48b.

                  TABLE 48b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          0         3                                            200 17 28                                                                      300 38 37                                                                      500 78 68                                                                     Formulation C 100  8 63                                                         200 43 96                                                                      300 88 96                                                                      500 99 98                                                                     Formulation J 100 12 10                                                         200 35 60                                                                      300 85 90                                                                      500 98 92                                                                     48-01 100 10  0                                                                 200 38 13                                                                      300 73 28                                                                      500 90 75                                                                     48-02 100  8  0                                                                 200 40 23                                                                      300 87 43                                                                      500 98 62                                                                     48-03 100 12  0                                                                 200 40 25                                                                      300 83 47                                                                      500 95 73                                                                     48-04 100  5  5                                                                 200 45 38                                                                      300 83 65                                                                      500 98 83                                                                     48-05 100 10  3                                                                 200 42 48                                                                      300 82 53                                                                      500 97 91                                                                     48-06 100 28  0                                                                 200 67 43                                                                      300 85 68                                                                      500 97 93                                                                     48-07 100  8  8                                                                 200 37 35                                                                      300 75 72                                                                      500 97 90                                                                     48-08 100  0  1                                                                 200 37 45                                                                      300 57 68                                                                      500 96 97                                                                     48-09 100  0  7                                                                 200 35 40                                                                      300 78 60                                                                      500 96 93                                                                     48-10 100  0  3                                                                 200 33 57                                                                      300 82 72                                                                      500 96 94                                                                     48-11 100  0  5                                                                 200 35 50                                                                      300 78 82                                                                      500 97 87                                                                     48-12 100  3  5                                                                 200 40 37                                                                      300 77 78                                                                      500 97 85                                                                     48-13 100  3  0                                                                 200 45 33                                                                      300 83 38                                                                      500 95 75                                                                     48-14 100  0  0                                                                 200 43 33                                                                      300 77 50                                                                      500 96 68                                                                     48-15 100  0  0                                                                 200 42 30                                                                      300 78 47                                                                      500 88 73                                                                   ______________________________________                                    

No great or consistent differences were seen with different orders of addition of ingredients.

Example 49

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 49a. Process (v) was followed for all compositions using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 49a                                                        ______________________________________                                         % w/w                                                                            Concentrate                                                                              Glyphosate      Fluorad                                                                              Fluorad                                        composition a.e. Lecithin FC-135 FC-754 MON 0818                             ______________________________________                                         49-01   15        4.0           8.0   0.5                                        49-02 15 6.0  8.0 0.5                                                          49-03 15 8.0  8.0 0.5                                                          49-04 10 4.0  8.0 0.5                                                          49-05 10 6.0  8.0 0.5                                                          49-06 10 8.0  8.0 0.5                                                          49-07 15 4.0 8.00  0.5                                                         49-08 15 6.0 8.00  0.5                                                         49-09 15 8.0 8.00  0.5                                                         49-10 15 6.0 8.25  0.5                                                         49-11 15 6.0 8.25  4.0                                                         49-12 15 8.0 4.00 4.0 0.5                                                      49-13 10 8.0 8.00  0.5                                                         49-14 10 8.0 4.00 4.0 0.5                                                    ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 22 days after planting ABUTH and 23 days after planting ECHCF, and evaluation of herbicidal inhibition was done 17 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 49b.

                  TABLE 49b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0        20                                            250 17 37                                                                      350 47 47                                                                      450 53 60                                                                     Formulation J 150 27 38                                                         250 68 80                                                                      350 78 95                                                                      450 87 95                                                                     49-01 150 15 30                                                                 250 78 68                                                                      350 97 87                                                                      450 97 78                                                                     49-02 150 47 30                                                                 250 92 80                                                                      350 97 97                                                                      450 98 85                                                                     49-03 150 30 35                                                                 250 83 45                                                                      350 97 57                                                                      450 97 67                                                                     49-04 150 47 32                                                                 250 80 57                                                                      350 95 87                                                                      450 97 96                                                                     49-05 150 32 30                                                                 250 81 89                                                                      350 94 95                                                                      450 98 94                                                                     49-06 150 60 28                                                                 250 80 96                                                                      350 92 95                                                                      450 98 96                                                                     49-07 150 50 23                                                                 250 70 72                                                                      350 92 78                                                                      450 97 60                                                                     49-08 150 45 40                                                                 250 72 72                                                                      350 90 89                                                                      450 97 77                                                                     49-09 150 53 25                                                                 250 80 78                                                                      350 89 89                                                                      450 96 93                                                                     49-10 150 72 48                                                                 250 89 83                                                                      350 98 95                                                                      450 98 80                                                                     49-11 150 50 27                                                                 250 77 63                                                                      350 93 83                                                                      450 97 72                                                                     49-12 150 52 15                                                                 250 83 57                                                                      350 94 68                                                                      450 98 63                                                                     49-13 150 50 30                                                                 250 75 32                                                                      350 88 84                                                                      450 97 77                                                                     49-14 150 67 23                                                                 250 84 77                                                                      350 97 73                                                                      450 97 72                                                                   ______________________________________                                    

In this test compositions prepared with Fluorad FC-754 tended to provide greater herbicidal effectiveness on ECHCF than their counterparts prepared with Fluorad FC-135.

Example 50

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 50a. Process (v) was followed for all compositions using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 50a                                                        ______________________________________                                         % w/w                                                                            Concentrate                                                                              Glypho-        Fluorad                                                                              Fluorad                                                                              MON  Iso-                                 composition sate a.e. Lecithin FC-135 FC-754 0818 propanol                   ______________________________________                                         50-01   15       6.0     8.25        4.0                                         50-02 15 6.0  8.25 4.0                                                         50-03 10 8.0 8.00  0.5                                                         50-04 10 8.0  8.00 0.5                                                         50-05 20 2.0 2.00  0.5                                                         50-06 20 2.0  2.00 0.5                                                         50-07 30 3.0 3.00  0.5                                                         50-08 30 3.0  3.00 0.5                                                         50-09 30 1.0 1.00  0.5                                                         50-10 30 1.0  1.00 0.5                                                         50-11 15 6.0 8.25  4.0 5.0                                                     50-12 15 6.0  8.25 4.0 5.0                                                     50-13 10 8.0 8.00  2.0 5.0                                                     50-14 10 8.0  8.00 2.0 5.0                                                     50-15 30 3.0  3.00 0.8                                                         50-16 30 3.0 3.00  0.8                                                         50-17 10 8.0 8.00  2.0 7.5                                                     50-18 10 8.0  8.00 2.0 7.5                                                     50-19 10 8.0 8.00  2.0 10.0                                                    50-20 10 8.0  8.00 2.0 10.0                                                    50-21 10 8.0 8.00  4.0 5.0                                                     50-22 10 8.0  8.00 4.0 5.0                                                   ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and 19 days after planting ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 50b.

                  TABLE 50b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          2        22                                            250 25 28                                                                      350 63 38                                                                      450 70 58                                                                     Formulation C 150 30 47                                                         250 75 82                                                                      350 97 97                                                                      450 100  99                                                                   Formulation J 150 10 43                                                         250 58 88                                                                      350 87 96                                                                      450 98 93                                                                     50-01 150 63 15                                                                 250 78 32                                                                      350 83 70                                                                     50-02 150 60 28                                                                 250 80 32                                                                      350 88 65                                                                     50-03 150 53 37                                                                 250 80 42                                                                      350 91 27                                                                     50-04 150 72 18                                                                 250 83 50                                                                      350 96 80                                                                     50-05 150 50  2                                                                 250 77 25                                                                      350 78 43                                                                     50-06 150 22 25                                                                 250 77 27                                                                      350 87 40                                                                     50-07 150 27 20                                                                 250 58 32                                                                      350 87 37                                                                     50-08 150 32  3                                                                 250 78 30                                                                      350 82 52                                                                     50-09 150  5  0                                                                 250 42 28                                                                      350 68 43                                                                     50-10 150  2 23                                                                 250 52 28                                                                      350 75 42                                                                     50-11 150 72 27                                                                 250 80 42                                                                      350 85 73                                                                     50-12 150 58 23                                                                 250 82 58                                                                      350 87 97                                                                     50-13 150 70  8                                                                 250 83 38                                                                      350 85 45                                                                     50-14 150 68 37                                                                 250 90 27                                                                      350 89 67                                                                     50-15 150 28 28                                                                 250 63 40                                                                      350 87 35                                                                     50-16 150 23 13                                                                 250 45 48                                                                      350 82 68                                                                     50-17 150 67  2                                                                 250 88 30                                                                      350 87 58                                                                     50-18 150 60 38                                                                 250 85 22                                                                      350 95 53                                                                     50-19 150 74 38                                                                 250 80 47                                                                      350 95 28                                                                     50-20 150 70 25                                                                 250 85 70                                                                      350 97 81                                                                     50-21 150 78  5                                                                 250 83 50                                                                      350 90 83                                                                     50-22 150 73 33                                                                 250 82 33                                                                      350 95 83                                                                   ______________________________________                                    

Concentrate compositions having a high (20-30% a.c.) loading of glyphosate and consequently a relatively low loading of excipients showed enhancement of herbicidal effectiveness over that obtained with Formulation B, but in this test did not provide efficacy equal to commercial standard Formulations C and J.

Example 51

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 51a. Process (i) was followed for compositions 51-13 to 51-20 and process (v) for compositions 51-01 to 51-12 using soybean lecithin (45% phospholipid, Avanti). Compositions were stored in different conditions as indicated below before testing for herbicidal effectiveness. The pH of all compositions was approximately 5.

                                      TABLE 51a                                    __________________________________________________________________________     % w/w                                                                          Concentrate                                                                          Glyphosate    Fluorad                                                                            Fluorad                                                                            MON                                                                               Storage                                           composition a.e. Lecithin LI-700 FC-135 FC-754 0818 conditions               __________________________________________________________________________     51-01 20.0  2.0         2.0 0.5                                                                               60° C., 4d                                 51-02 15.0 6.0  8.25  4.0 60° C., 4 d                                   51-03 20.0 2.0   2.0 0.5 -10° C., 4 d                                   51-04 15.0 6.0  8.25  4.0 -10° C., 4 d                                  51-05 20.0 2.0   2.0 0.5 room temperature, 4 d                                 51-06 15.0 6.0  8.25  4.0 room temperature, 4 d                                51-07 20.0 2.0   2.0 0.5 60° C., 8 h then -10° C., 4 d                                         51-08 15.0 6.0  8.25  4.0 60° C.,                                      8 h then -10° C., 4 d                      51-09 20.0 2.0   2.0 0.5 freshly made                                          51-10 15.0 6.0  8.25  4.0 freshly made                                         51-11 20.0 2.0   2.0 0.5 room temperature,42 d                                 51-12 15.0 6.0  8.25  4.0 room temperature, 42 d                               51-13 15.0  18.25                                                              51-14 20.0  4.50                                                               51-15 15.0  14.25    4.0                                                       51-16 20.0  4.00   0.5                                                         51-17 15.0  10.00  8.25                                                        51-18 20.0  2.50  2.0                                                          51-19 15.0  6.00 8.25  4.0                                                     51-20 20.0  2.00 2.00  0.5                                                   __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and 18 days after planting ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 51b.

                  TABLE 51b                                                        ______________________________________                                                    Glyphosate rate                                                                          % Inhibition                                              Spray composition                                                                           g a.e./ha   ABUTH      ECHCF                                      ______________________________________                                         Formulation B                                                                               150         27         30                                            250 37 38                                                                      350 60 42                                                                      450 69 45                                                                     Formulation J 150 45 61                                                         250 81 92                                                                      350 93 97                                                                      450 96 97                                                                     51-01 150 45 25                                                                 250 49 41                                                                      350 66 47                                                                      450 75 63                                                                     51-02 150 49 65                                                                 250 74 67                                                                      350 83 88                                                                      450 92 87                                                                     51-03 150 32 25                                                                 250 71 70                                                                      350 75 65                                                                      450 77 67                                                                     51-04 150 54 68                                                                 250 82 82                                                                      350 91 95                                                                      450 87 96                                                                     51-05 150 39 52                                                                 250 63 65                                                                      350 83 90                                                                      450 85 93                                                                     51-06 150 67 81                                                                 250 89 97                                                                      350 94 100                                                                     450 96 100                                                                    51-07 150 39 52                                                                 250 60 88                                                                      350 87 94                                                                      450 85 96                                                                     51-08 150 54 82                                                                 250 87 98                                                                      350 93 100                                                                     450 92 100                                                                    51-09 150 45 53                                                                 250 67 88                                                                      350 84 89                                                                      450 93 93                                                                     51-10 150 56 63                                                                 250 86 97                                                                      350 94 99                                                                      450 92 98                                                                     51-11 150 48 40                                                                 250 69 55                                                                      350 74 91                                                                     51-12 150 60 41                                                                 250 86 91                                                                      350 95 98                                                                     51-13 150 30 44                                                                 250 37 76                                                                      350 59 94                                                                     51-14 150  0 40                                                                 250 49 55                                                                      350 59 85                                                                     51-15 150 42 61                                                                 250 71 90                                                                      350 83 97                                                                     51-16 150 27 42                                                                 250 49 58                                                                      350 61 86                                                                     51-17 150 37 45                                                                 250 52 70                                                                      350 76 60                                                                     51-18 150 28 32                                                                 250 53 77                                                                      350 70 71                                                                     51-19 150 47 36                                                                 250 69 97                                                                      350 83 89                                                                     51-20 150 26 20                                                                 250 56 74                                                                      350 62 82                                                                   ______________________________________                                    

No great or consistent effect of storage conditions on herbicidal effectiveness of compositions was seen in this test.

Example 52

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 52a. Process (v) was followed for all compositions using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                                      TABLE 52a                                    __________________________________________________________________________     % w/w                                                                          Concentrate                                                                          Glyphosate                                                                               Butyl                                                                              Fluorad                                                                            MON                                                                               Ethomeen                                              composition a.e. Lecithin stearate FC-754 0818 T/25 Ethanol                  __________________________________________________________________________     52-01 20    2.0 0.5        1.25 1.0                                              52-02 20 2.0 0.5  1.00 1.00 1.0                                                52-03 20 2.0 0.5  1.25  1.0                                                    52-04 20 6.0 1.5   3.00 3.0                                                    52-05 20 6.0 1.5  2.00 2.00 2.0                                                52-06 20 6.0 1.5  3.00  3.0                                                    52-07 20 2.0 0.5   0.50                                                        52-08 20 2.0 0.5   2.50                                                        52-09 20 2.0 0.5  1.25 1.25                                                    52-10 20 6.0 1.5   0.50                                                        52-11 20 6.0 1.5   3.00                                                        52-12 20 6.0 1.5   6.00                                                        52-13 20 6.0 1.5  3.00 3.00                                                    52-14 20 2.0  2.0 0.50                                                         52-15 20 6.0  3.0 6.00                                                         52-16 20 6.0  6.0 6.00                                                       __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulation J was applied as a comparative treatment. Results, averaged for all replicates of each treatment, are shown in Table 52b.

                  TABLE 52b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation J 150         38        45                                            250 80 63                                                                      350 78 82                                                                      450 75 55                                                                     52-01 150 23 27                                                                 250 57 53                                                                      350 70 85                                                                      450 70 83                                                                     52-02 150  7 25                                                                 250 52 45                                                                      350 82 88                                                                      450 82 90                                                                     52-03 150 38 35                                                                 250 50 40                                                                      350 82 92                                                                      450 83 93                                                                     52-04 150 40 48                                                                 250 73 75                                                                      350 78 92                                                                      450 88 92                                                                     52-05 150 50 53                                                                 250 68 80                                                                      350 85 98                                                                      450 89 96                                                                     52-06 150 50 43                                                                 250 55 80                                                                      350 78 97                                                                      450 85 91                                                                     52-07 150  3 28                                                                 250 22 43                                                                      350 67 72                                                                      450 73 75                                                                     52-08 150 43 33                                                                 250 77 63                                                                      350 89 78                                                                      450 97 85                                                                     52-09 150 57 27                                                                 250 95 63                                                                      350 89 86                                                                      450 98 88                                                                     52-10 150 32 23                                                                 250 33 55                                                                      350 73 82                                                                      450 67 60                                                                     52-11 150 45 32                                                                 250 78 72                                                                      350 95 92                                                                      450 98 96                                                                     52-12 150 67 42                                                                 250 80 75                                                                      350 96 88                                                                      450 97 90                                                                     52-13 150 73 42                                                                 250 83 77                                                                      350 96 91                                                                      450 98 88                                                                     52-14 150 57 30                                                                 250 77 72                                                                      350 84 80                                                                      450 96 75                                                                     52-15 150 72 38                                                                 250 88 82                                                                      350 98 92                                                                      450 98 87                                                                     52-16 150 85 49                                                                 250 97 47                                                                      350 97 83                                                                      450 98 85                                                                   ______________________________________                                    

Very high herbicidal effectiveness was obtained in this test with concentrate compositions containing lecithin and Fluorad FC-754. Composition 52-14, containing each of these excipients at the very low weight/weight ratio to glyphosate a.e. of 1:10, was at least as effective as commercial standard Formulation J, while compositions 52-15 and 52-16 were still more effective. Also performing very well in this test, particularly on ECHCF, were a number of concentrate compositions containing lecithin and butyl stearate.

Example 53

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 53a. Process (v) was followed for all compositions using soybean lecithin (45% phospholipid, Avanti). Order of addition of ingredients was varied for certain compositions as indicated below. The pH of all compositions was approximately 5.

                                      TABLE 53a                                    __________________________________________________________________________                 % w/w                 Order of                                     Concentrate                                                                          Glyphosate                                                                               Fluorad                                                                              Benzalk-                                                                            Butyl                                                                              MON                                                                               addition                                       composition g/l a.e. Lecithin FC-754/135 onium Cl stearate 0818              __________________________________________________________________________                                       (*)                                          53-01 345   4.0       0.66                                                       53-02 345 4.0  1.00                                                            53-03 347 3.0  3.00                                                            53-04 347 4.0  4.00                                                            53-05 347 4.0  5.00                                                            53-06 345 4.6  4.60                                                            53-07 348 4.0 2.0 (754) 1.10                                                   53-08 351 4.0 4.0 (754) 1.00   A                                               53-09 346 3.9 4.2 (754) 1.00   B                                               53-10 350 4.0 2.0 (135) 1.10                                                   53-11 352 4.0 4.0 (135) 1.00   A                                               53-12 349 4.0 4.0 (135) 1.00   B                                               53-13 348 4.0 4.0 (754) 0.50 0.57                                              53-14 347 4.0  0.50 0.52                                                       53-15 348 3.7  0.48  3.7                                                       53-16 348 4.0  0.58  4.0                                                     __________________________________________________________________________

(*) Order of addition:

    ______________________________________                                         1st      2nd       3rd        4th     5th                                      ______________________________________                                         A   lecithin water     Benzalkonium                                                                            FC-135/754                                                                             glyphosate                                  Cl                                                                          B glyphosate FC-135/754 Benzalkonium water glyphosate                             Cl                                                                        ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 21 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 53b.

                  TABLE 53b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          5         5                                            200 15 20                                                                      300 47 30                                                                      400 65 37                                                                     Formulation J 100  0  8                                                         200 70 37                                                                      300 78 70                                                                      400 83 73                                                                     53-01 100  3 10                                                                 200 17 27                                                                      300 45 37                                                                      400 75 40                                                                     53-02 100  2  5                                                                 200 13 30                                                                      300 43 40                                                                      400 75 47                                                                     53-03 100  0  8                                                                 200 17 43                                                                      300 65 78                                                                      400 78 83                                                                     53-04 100  2 10                                                                 200 30 37                                                                      300 68 72                                                                      400 75 88                                                                     53-05 100  2 20                                                                 200 25 65                                                                      300 63 88                                                                      400 82 83                                                                     53-06 100 10 17                                                                 200 25 33                                                                      300 47 77                                                                      400 83 75                                                                     53-07 100  0 10                                                                 200 48 30                                                                      300 73 37                                                                      400 83 43                                                                     53-08 100  3 10                                                                 200 33 30                                                                      300 68 37                                                                      400 78 40                                                                     53-09 100  5 10                                                                 200 40 27                                                                      300 65 50                                                                      400 70 57                                                                     53-10 100  0 10                                                                 200 30 27                                                                      300 67 40                                                                      400 73 40                                                                     53-11 100  0 10                                                                 200 33 27                                                                      300 52 37                                                                      400 82 40                                                                     53-12 100  0 10                                                                 200 40 20                                                                      300 65 40                                                                      400 72 40                                                                     53-13 100  0 10                                                                 200 40 20                                                                      300 60 33                                                                      400 78 33                                                                     53-14 100  0 10                                                                 200  7 47                                                                      300 28 33                                                                      400 43 43                                                                     53-15 100  0 13                                                                 200 27 33                                                                      300 73 53                                                                      400 77 67                                                                     53-16 100  0 13                                                                 200 30 37                                                                      300 75 47                                                                      400 77 68                                                                   ______________________________________                                    

Most concentrate compositions of this Example showed enhanced glyphosate effectiveness by comparison with Formulation B but did not equal the efficacy of commercial standard Formulation J in this test.

Example 54

Aqueous spray and concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 54a. Process (i) was followed for spray compositions 54-37 to 54-60 and process (iii) for spray compositions 54-01 to 54-36 using soybean lecithin (45% phospholipid, Avanti). Process (v) was followed for concentrate compositions 54-61 to 54-63 using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 54a                                                        ______________________________________                                         Glyphosate    % w/w          Type of                                           Composition                                                                            g a.e./l  Lecithin                                                                               Fluoro-organic                                                                          fluoro-organic                              ______________________________________                                         Spray composition                                                                54-01     1.60      0.027 0.027    Fluorad FC-754                              54-02 2.66 0.045 0.045 Fluorad FC-754                                          54-03 3.72 0.062 0.062 Fluorad FC-754                                          54-04 4.79 0.080 0.080 Fluorad FC-754                                          54-05 1.60 0.027 0.027 Fluorad FC-750                                          54-06 2.66 0.045 0.045 Fluorad FC-750                                          54-07 3.72 0.062 0.062 Fluorad FC-750                                          54-08 4.79 0.080 0.080 Fluorad FC-750                                          54-09 1.60 0.027 0.027 Fluorad FC-751                                          54-10 2.66 0.045 0.045 Fluorad FC-751                                          54-11 3.72 0.062 0.062 Fluorad FC-751                                          54-12 4.79 0.080 0.080 Fluorad FC-751                                          54-13 1.60 0.027 0.027 Fluorad FC-760                                          54-14 2.66 0.045 0.045 Fluorad FC-760                                          54-15 3.72 0.062 0.062 Fluorad FC-760                                          54-16 4.79 0.080 0.080 Fluorad FC-760                                          54-17 1.60 0.027 0.027 Fluorad FC-120                                          54-18 2.66 0.045 0.045 Fluorad FC-120                                          54-19 3.72 0.062 0.062 Fluorad FC-120                                          54-20 4.79 0.080 0.080 Fluorad FC-120                                          54-21 1.60 0.027 0.027 Fluorad FC-171                                          54-22 2.66 0.045 0.045 Fluorad FC-171                                          54-23 3.72 0.062 0.062 Fluorad FC-171                                          54-24 4.79 0.080 0.080 Fluorad FC-171                                          54-25 1.60 0.027 0.027 Fluorad FC-129                                          54-26 2.66 0.045 0.045 Fluorad FC-129                                          54-27 3.72 0.062 0.062 Fluorad FC-129                                          54-28 4.79 0.080 0.080 Fluorad FC-129                                          54-29 1.60 0.027 0.027 Fluorad FC-170C                                         54-30 2.66 0.045 0.045 Fluorad FC-170C                                         54-31 3.72 0.062 0.062 Fluorad FC-170C                                         54-32 4.79 0.080 0.080 Fluorad FC-170C                                         54-33 1.60  0.027 Fluorad FC-754                                               54-34 2.66  0.045 Fluorad FC-754                                               54-35 3.72  0.062 Fluorad FC-754                                               54-36 4.79  0.080 Fluorad FC-754                                               54-37 1.60  0.027 Fluorad FC-750                                               54-38 2.66  0.045 Fluorad FC-750                                               54-39 3.72  0.062 Fluorad FC-750                                               54-40 4.79  0.080 Fluorad FC-750                                               54-41 1.60  0.027 Fluorad FC-760                                               54-42 2.66  0.045 Fluorad FC-760                                               54-43 3.72  0.062 Fluorad FC-760                                               54-44 4.79  0.080 Fluorad FC-760                                               54-45 1.60  0.027 Fluorad FC-120                                               54-46 2.66  0.045 Fluorad FC-120                                               54-47 3.72  0.062 Fluorad FC-120                                               54-48 4.79  0.080 Fluorad FC-120                                               54-49 1.60  0.027 Fluorad FC-171                                               54-50 2.66  0.045 Fluorad FC-171                                               54-51 3.72  0.062 Fluorad FC-171                                               54-52 4.79  0.080 Fluorad FC-171                                               54-53 1.60  0.027 Fluorad FC-129                                               54-54 2.66  0.045 Fluorad FC-129                                               54-55 3.72  0.062 Fluorad FC-129                                               54-56 4.79  0.080 Fluorad FC-129                                               54-57 1.60  0.027 Fluorad FC-170C                                              54-58 2.66  0.045 Fluorad FC-170C                                              54-59 3.72  0.062 Fluorad FC-170C                                              54-60 4.79  0.080 Fluorad FC-170C                                            Concentrate compositions:                                                        54-61     180       1.5   1.5      Fluorad FC-754                              54-62 180 2.5 2.5 Fluorad FC-754                                               54-63 180 3.0 6.0 Fluorad FC-754                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and 19 days after planting ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B and J were applied as a comparative treatment. Results, averaged for all replicates of each treatment, are shown in Table 54b.

                  TABLE 54b                                                        ______________________________________                                                        Glyphosate rate                                                                         % Inhibition                                           Spray or concentrate composition                                                                g a.e./ha  ABUTH    ECHCF                                     ______________________________________                                         Formulation B    150        47       88                                           250 68 96                                                                      350 86 98                                                                      450 93 100                                                                    Formulation J 150 68 89                                                         250 94 97                                                                      350 98 100                                                                     450 100  99                                                                   54-01 150 94 83                                                                54-02 250 97 99                                                                54-03 350 97 99                                                                54-04 450 99 100                                                               54-05 150 93 77                                                                54-06 250 94 96                                                                54-07 350 97 94                                                                54-08 450 98 99                                                                54-09 150 53 72                                                                54-10 250 68 86                                                                54-11 350 73 99                                                                54-12 450 91 96                                                                54-13 150 58 70                                                                54-14 250 72 94                                                                54-15 350 89 95                                                                54-16 450 93 92                                                                54-17 150 50 62                                                                54-18 250 58 78                                                                54-19 350 85 93                                                                54-20 450 84 96                                                                54-21 150 53 63                                                                54-22 250 83 85                                                                54-23 350 89 90                                                                54-24 450 96 86                                                                54-25 150 53 57                                                                54-26 250 78 85                                                                54-27 350 90 91                                                                54-28 450 96 93                                                                54-29 150 62 70                                                                54-30 250 84 92                                                                54-31 350 97 97                                                                54-32 450 97 98                                                                54-33 150 94 79                                                                54-34 250 96 97                                                                54-35 350 97 99                                                                54-36 450 98 99                                                                54-37 150 90 84                                                                54-38 250 99 96                                                                54-39 350 98 100                                                               54-40 450 99 100                                                               54-41 150 68 75                                                                54-42 250 73 88                                                                54-43 350 83 92                                                                54-44 450 92 98                                                                54-45 150 48 53                                                                54-46 250 60 88                                                                54-47 350 82 97                                                                54-48 450 95 95                                                                54-49 150 50 47                                                                54-50 250 63 89                                                                54-51 350 83 91                                                                54-52 450 91 90                                                                54-53 150 48 52                                                                54-54 250 63 75                                                                54-55 350 91 92                                                                54-56 450 97 97                                                                54-57 150 50 83                                                                54-58 250 73 94                                                                54-59 350 91 98                                                                54-60 450 94 98                                                                54-61 150 63 52                                                                 250 96 96                                                                      350 97 96                                                                     54-62 150 77 77                                                                 250 93 87                                                                      350 98 98                                                                     54-63 150 83 89                                                                 250 96 96                                                                      350 98 98                                                                   ______________________________________                                    

Outstanding herbicidal efficacy, even by comparison with Formulation J, was obtained in this test from spray compositions containing lecithin and Fluorad FC-754 (54-01 to 54-04). Substitution of other fluoro-organic surfactants for Fluorad FC-754 gave varying results. Fluorad FC-750 (compositions 54-05 to 54-08) was an acceptable substitute; however Fluorad FC-751, Fluorad FC-760, Fluorad FC-120, Fluorad FC-171, Fluorad FC-129 and Fluorad FC-170C (compositions 54-09 to 54-32) provided less enhancement. A similar pattern was seen with spray compositions (54-33 to 54-60) containing the same fluoro-organic surfactants as above with the exception of Fluorad FC-751, but no lecithin. It is noteworthy that of all the fluoro-organic surfactants included in this test, only Fluorad FC-754 and Fluorad FC-750 are cationic. Excellent herbicidal efficacy was also noted in this test from concentrate glyphosate compositions containing lecithin and Fluorad FC-754, especially composition 54-63.

Example 55

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 55a. Concentrate compositions 55-01 to 55-07, 55-17 and 55-18 were prepared by process (v). Concentrate compositions 55-08 to 55-15 were prepared by process (x). The other concentrate compositions of this Example were included for comparison purposes.

                                      TABLE 55a                                    __________________________________________________________________________               % w/w                                                                Conc.                                                                              Glyphosate                                                                               Fluorad                                                                            Butyl                                                                              Ethomeen   Arcosolve                                       comp. g a.e./1 Lecithin FC-754 stearate T/25 Ceteareth-20 DPM Ceteareth-                                           27                                       __________________________________________________________________________     55-01                                                                              348   3.0 3.00    0.75                                                       55-02 348 3.8 3.75  5.00                                                       55-03 348 3.8 3.75  7.50                                                       55-04 348 2.0 5.00  0.75                                                       55-05 348 5.0 5.00  0.75                                                       55-06 348 2.0 2.00                                                             55-07 348 1.0 1.00                                                             55-08 220 1.5  1.5 3.00 3.0                                                    55-09 220 1.5  1.5 3.00   3.0                                                  55-10 220 1.5  1.5 6.00 3.0                                                    55-11 220 1.5  1.5 6.00   3.0                                                  55-12 220 3.0  1.5 3.00 3.0                                                    55-13 220 3.0  1.5 3.00   3.0                                                  55-14 348 1.5  1.5 6.00 3.0                                                    55-15 348 3.0  1.5 3.00 3.0                                                    55-16 348  3.00                                                                55-17 348 3.0     3.0                                                          55-18 348 5.0   13.00    5.0                                                 __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 55b.

                  TABLE 55b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         28        32                                            200 41 37                                                                      300 73 64                                                                      400 22 30                                                                     Formulation J 100 38 32                                                         200 82 73                                                                      300 89 91                                                                      400 97 89                                                                     55-01 100 73 28                                                                 200 90 66                                                                      300 97 92                                                                      400 100   96                                                                  55-02 100 77 32                                                                 200 87 67                                                                      300 84 78                                                                      400 98 84                                                                     55-03 100 79 33                                                                 200 82 66                                                                      300 99 81                                                                      400 97 88                                                                     55-04 100 69 35                                                                 200 95 59                                                                      300 96 84                                                                      400 92 91                                                                     55-05 100 82 32                                                                 200 92 55                                                                      300 96 71                                                                      400 94 87                                                                     55-06 100 83 33                                                                 200 100  52                                                                    300 100  68                                                                    400 99 75                                                                     55-07 100 77 35                                                                 200 90 58                                                                      300 95 71                                                                      400 94 90                                                                     55-08 100 51 40                                                                 200 89 75                                                                      300 96 92                                                                      400 95 98                                                                     55-09 100 76 57                                                                 200 98 81                                                                      300 97 86                                                                      400 96 98                                                                     55-10 100 69 60                                                                 200 98 63                                                                      300 95 82                                                                      400 99 90                                                                     55-11 100 61 60                                                                 200 94 84                                                                      300 97 89                                                                      400 99 97                                                                     55-12 100 64 53                                                                 200 95 82                                                                      300 96 90                                                                      400 95 98                                                                     55-13 100 61 58                                                                 200 94 78                                                                      300 88 87                                                                      400 100  94                                                                   55-14 100 56 61                                                                 200 88 77                                                                      300 91 82                                                                      400 97 89                                                                     55-15 100 42 52                                                                 200 82 80                                                                      300 86 90                                                                      400 97 92                                                                     55-16 100 64 49                                                                 200 86 75                                                                      300 97 88                                                                      400 100  82                                                                   55-17 100 57 32                                                                 200 88 66                                                                      300 95 73                                                                      400 100  88                                                                   55-18 100 52 35                                                                 200 70 77                                                                      300 82 79                                                                      400 97 73                                                                   ______________________________________                                    

Concentrate compositions 55-01 to 55-07, containing lecithin and Fluorad FC-754, exhibited outstanding herbicidal effectiveness. On ABUTH, several of these were about as effective at 100 g a.e./ha as commercial standard Formulation J at 200 g a.e./ha. On ECHCF, all exhibited strong enhancement over Formulation B but most did not equal Formulation J on this species. The performance of composition 55-07, containing lecithin and Fluorad FC-754 each at the extremely low weight/weight ratio to glyphosate a.e. of about 1:30, was remarkably high. The inclusion of a relatively high concentration of Ethomeen T/25, as in compositions 55-02 and 55-03, was not helpful to herbicidal effectiveness in the presence of lecithin and Fluorad FC-754, and may even have been detrimental. The relatively poor performance of composition 55-18, having a high Ethomeen T/25 concentration but in this case no Fluorad FC-754, is consistent with this observation. Without being bound by theory, it is believed that the presence of such high concentrations of Ethomeen T/25 together with lecithin results in the formation of mixed micelles rather than liposomes in aqueous dispersion. Composition 55-16, containing Fluorad FC-754 at a weight/weight ratio to glyphosate a.e. of about 1:10, but no lecithin, exhibited herbicidal effectiveness similar to that of composition 55-01, suggesting that under the conditions of this test a large part of the enhancement due to the lecithin/Fluorad FC-754 combination was attributable to the Fluorad FC-754 component.

Compositions 55-08 to 55-15, containing lecithin, butyl stearate, Ethomeen T/25 and a C₁₆₋₁₈ alkylether surfactant (ceteareth-20 or ceteareth-27) exhibited a very high degree of herbicidal effectiveness. Not only was performance, at least of 55-08 to 55-13, on ABUTH substantially better than that of Formulation J, these compositions performed considerably better than Formulation J on ECHCF as well.

Example 56

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 56a. Process (i) was followed for compositions 56-61 to 56-64, 56-67, 56-69 and 56-71 and process (iii) for compositions 56-01 to 56-66, 56-68, 56-70 and 56-72 using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 56a                                                        ______________________________________                                         % w/w                                                                            Spray                     Fluorad                                                                              Ethomeen                                                                              Ethomeen                                composition Lecithin MON 0818 FC-754 T/25 C/12                               ______________________________________                                         56-01   0.020   0.025     0.02                                                   56-02 0.030 0.025 0.02                                                         56-03 0.050 0.025 0.02                                                         56-04 0.020 0.025 0.03                                                         56-05 0.030 0.025 0.03                                                         56-06 0.050 0.025 0.03                                                         56-07 0.020 0.025 0.04                                                         56-08 0.030 0.025 0.04                                                         56-09 0.050 0.025 0.04                                                         56-10 0.020 0.025 0.05                                                         56-11 0.030 0.025 0.05                                                         56-12 0.050 0.025 0.05                                                         56-13 0.020  0.02                                                              56-14 0.030  0.02                                                              56-15 0.050  0.02                                                              56-16 0.020  0.03                                                              56-17 0.030  0.03                                                              56-18 0.050  0.03                                                              56-19 0.020  0.04                                                              56-20 0.030  0.04                                                              56-21 0.050  0.04                                                              56-22 0.020  0.05                                                              56-23 0.030  0.05                                                              56-24 0.050  0.05                                                              56-25 0.020  0.02 0.025                                                        56-26 0.030  0.02 0.025                                                        56-27 0.050  0.02 0.025                                                        56-28 0.020  0.03 0.025                                                        56-29 0.030  0.03 0.025                                                        56-30 0.050  0.03 0.025                                                        56-31 0.020  0.04 0.025                                                        56-32 0.030  0.04 0.025                                                        56-33 0.050  0.04 0.025                                                        56-34 0.020  0.05 0.025                                                        56-35 0.030  0.05 0.025                                                        56-36 0.050  0.05 0.025                                                        56-37 0.020  0.02  0.025                                                       56-38 0.030  0.02  0.025                                                       56-39 0.050  0.02  0.025                                                       56-40 0.020  0.03  0.025                                                       56-41 0.030  0.03  0.025                                                       56-42 0.050  0.03  0.025                                                       56-43 0.020  0.04  0.025                                                       56-44 0.030  0.04  0.025                                                       56-45 0.050  0.04  0.025                                                       56-46 0.020  0.05  0.025                                                       56-47 0.030  0.05  0.025                                                       56-48 0.050  0.05  0.025                                                       56-49 0.020  0.02 0.050                                                        56-50 0.025  0.03 0.050                                                        56-51 0.050  0.02 0.050                                                        56-52 0.020  0.03 0.050                                                        56-53 0.030  0.03 0.050                                                        56-54 0.050  0.03 0.050                                                        56-55 0.020 0.050 0.02                                                         56-56 0.025 0.050 0.03                                                         56-57 0.050 0.050 0.02                                                         56-58 0.020 0.050 0.03                                                         56-59 0.030 0.050 0.03                                                         56-60 0.050 0.050 0.03                                                         56-61  0.050                                                                   56-62    0.050                                                                 56-63     0.025                                                                56-64  0.025                                                                   56-65 0.050  0.08 0.025                                                        56-66 0.025  0.03  0.025                                                       56-67   0.05                                                                   56-68 0.050                                                                    56-69   0.05 0.050                                                             56-70 0.050   0.050                                                            56-71  0.050 0.05                                                              56-72 0.050 0.050                                                            ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulation J was applied as a comparative treatment. Results, averaged for all replicates of each treatment, are shown in Table 56b.

                  TABLE 56b                                                        ______________________________________                                                   Glyphosate rate                                                                           % Inhibition                                              Spray composition                                                                          g a.e./ha    ABUTH     ECHCF                                       ______________________________________                                         Formulation J                                                                              100          14        42                                             187 44 87                                                                      300 71 90                                                                      400 92 97                                                                     56-01 187 80 80                                                                56-02 187 80 97                                                                56-03 187 79 94                                                                56-04 187 79 91                                                                56-05 187 81 80                                                                56-06 187 73 88                                                                56-07 187 86 90                                                                56-08 187 88 91                                                                56-09 187 77 85                                                                56-10 187 81 80                                                                56-11 187 88 68                                                                56-12 187 87 72                                                                56-13 187 85 61                                                                56-14 187 83 47                                                                56-15 187 86 61                                                                56-16 187 86 57                                                                56-17 187 85 44                                                                56-18 187 81 62                                                                56-19 187 82 63                                                                56-20 187 87 62                                                                56-21 187 84 48                                                                56-22 187 80 67                                                                56-23 187 86 89                                                                56-24 187 78 64                                                                56-25 187 84 87                                                                56-26 187 81 81                                                                56-27 187 74 85                                                                56-28 187 71 90                                                                56-29 187 76 74                                                                56-30 187 81 89                                                                56-31 187 78 80                                                                56-32 187 79 84                                                                56-33 187 82 84                                                                56-34 187 74 87                                                                56-35 187 81 89                                                                56-36 187 85 79                                                                56-37 187 68 89                                                                56-38 187 69 85                                                                56-39 187 86 85                                                                56-40 187 83 89                                                                56-41 187 77 76                                                                56-42 187 83 76                                                                56-43 187 74 83                                                                56-44 187 84 69                                                                56-45 187 85 71                                                                56-46 187 80 86                                                                56-47 187 83 96                                                                56-48 187 81 87                                                                56-49 187 75 99                                                                56-50 187 78 97                                                                56-51 187 76 97                                                                56-52 187 77 92                                                                56-53 187 74 88                                                                56-54 187 73 81                                                                56-55 187 70 87                                                                56-56 187 79 88                                                                56-57 187 72 89                                                                56-58 187 72 79                                                                56-59 187 53 80                                                                56-60 187 80 73                                                                56-61 187 46 78                                                                56-62 187 54 94                                                                56-63 187 48 98                                                                56-64 187 59 97                                                                56-65 187 87 84                                                                56-66 187 89 96                                                                56-67 187 86 69                                                                56-68 187 46 43                                                                56-69 187 75 90                                                                56-70 187 55 83                                                                56-71 187 79 80                                                                56-72 187 55 82                                                              ______________________________________                                    

All compositions of this Example containing Fluorad FC-754 showed much greater herbicidal effectiveness on ABUTH at 187 g a.e./ha than did Formulation J at the same rate, in many cases giving inhibition of ABUTH equal to or greater than provided by Formulation J at 300 g a.e./ha. The only compositions of the Example not showing strong improvement over Formulation J on ABUTH were 56-61 to 56-64, 56-68, 56-70 and 56-72. These are the only formulations of the Example not containing Fluorad FC-754.

Example 57

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 57a. Process (i) was followed for compositions 57-02, 57-04, 57-06, 57-08, 57-10, 57-12, 57-14 and 57-16 to 57-18, and compositions 57-01, 57-03, 57-05, 57-07, 57-09, 57-11 and 57-13 using soybean lecithin (45% phospholipid, Avanti). The pH of all compositions was approximately 5.

                  TABLE 57a                                                        ______________________________________                                         Spray       % w/w               Type of                                        composition Lecithin                                                                               Surfactant  surfactant                                     ______________________________________                                         57-01       0.05    0.05        Surf H2                                          57-02  0.05 Surf H2                                                            57-03 0.05 0.05 Surf H3                                                        57-04  0.05 Surf H3                                                            57-05 0.05 0.05 Surf H4                                                        57-06  0.05 Surf H4                                                            57-07 0.05 0.05 Surf H5                                                        57-08  0.05 Surf H5                                                            57-09 0.05 0.05 Fluorad FC-754                                                 57-10  0.05 Fluorad FC-754                                                     57-11 0.05 0.05 Surf H1                                                        57-12  0.05 Surf H1                                                            57-13 0.05 0.05 MON 0818                                                       57-14  0.05 MON 0818                                                           57-15 0.05 0.05 Ethomeen T/25                                                  57-16  0.05 Ethomeen T/25                                                      57-17  0.10 MON 0818                                                           57-18  0.10 Ethomeen T/25                                                    ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 57b.

                  TABLE 57b                                                        ______________________________________                                                   Glyphosate rate                                                                           % Inhibition                                              Spray composition                                                                          g a.e./ha    ABUTH     ECHCF                                       ______________________________________                                         Formulation B                                                                              100          12        22                                             200 43 43                                                                      300 63 78                                                                      400 75 82                                                                     Formulation J 100 47 27                                                         200 89 83                                                                      300 98 98                                                                      400 99 97                                                                     57-01 100 65 60                                                                 200 94 84                                                                      300 99 97                                                                      400 100   98                                                                  57-02 100 40 45                                                                 200 77 75                                                                      300 91 90                                                                      400 94 98                                                                     57-03 100 63 37                                                                 200 82 82                                                                      300 97 99                                                                      400 99 97                                                                     57-04 100 52 38                                                                 200 79 73                                                                      300 95 98                                                                      400 99 97                                                                     57-05 100 73 68                                                                 200 85 94                                                                      300 98 99                                                                      400 100  99                                                                   57-06 100 38 58                                                                 200 73 92                                                                      300 85 100                                                                     400 100  98                                                                   57-07 100 50 43                                                                 200 80 78                                                                      300 94 86                                                                      400 94 95                                                                     57-08 100 50 48                                                                 200 75 62                                                                      300 89 77                                                                      400 90 79                                                                     57-09 100 91 47                                                                 200 98 75                                                                      300 99 97                                                                      400 99 94                                                                     57-10 100 87 38                                                                 200 89 73                                                                      300 99 83                                                                      400 100  94                                                                   57-11 100 77 73                                                                 200 93 79                                                                      300 98 96                                                                      400 99 98                                                                     57-12 100 55 52                                                                 200 82 89                                                                      300 96 99                                                                      400 99 100                                                                    57-13 100 75 63                                                                 200 93 92                                                                      300 98 99                                                                      400 99 99                                                                     57-14 100 78 82                                                                 200 88 86                                                                      300 96 99                                                                      400 99 100                                                                    57-15 100 77 68                                                                 200 94 95                                                                      300 98 97                                                                      400 99 98                                                                     57-16 100 75 75                                                                 200 88 99                                                                      300 98 99                                                                      400 99 100                                                                    57-17 100 72 77                                                                 200 85 98                                                                      300 98 100                                                                     400 99 99                                                                     57-18 100 77 77                                                                 200 90 96                                                                      300 97 99                                                                      400 99 100                                                                  ______________________________________                                    

Herbicidal activity with compositions 57-13 to 57-18, based on alkylamine based surfactants known in the art, was very high in this test. Compositions 57-01 to 57-12 of the present invention also exhibited excellent herbicidal effectiveness. Overall, surfactants "Surf H1" to "Surf H5" having hydrocarbon hydrophobes were not quite as effective as Fluorad FC-754 having a fluorocarbon hydrophobe, either when used as sole excipient substance or together with lecithin.

Example 58

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 58a. These compositions are water-in-oil-in-water multiple emulsions and were prepared by process (vi) described above.

                                      TABLE 58a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                           Butyl                                                                              Emulsifier                                                                          Emulsifier                                                                          % in inner aq. phase                                                                     Emulsifier                                                                           Emulsifier                             comp.                                                                              a.e.  stearate                                                                           #1   #2   Water                                                                              Glyphosate                                                                           #1    #2                                     __________________________________________________________________________     58-01                                                                              10    18.0                                                                               3.0   5.0 9.0 20    Span 80                                                                              Tween 20                                 58-02 10 7.5 3.0  5.0 4.5 20  Span 80 Tween 20                                 58-03 10 7.5 3.0 10.0 4.5 0 Surfynol 104 Neodol 25-12                          58-04 10 7.5 3.0 10.0 4.5 0 Surfynol 104 Neodol 25-20                          58-05 10 7.5 3.0 10.0 4.5 0 Surfynol 104 Tergitol 15-S-15                      58-06 10 7.5 3.0 10.0 4.5 0 Surfynol 104 Tergitol 15-S-20                      58-07 10 7.5 3.0 10.0 4.5 0 Surfynol 104 Tween 20                              58-08 10 7.5 3.0 10.0 4.5 0 Surfynol 104 ceteareth-55                          58-09 10 7.5 3.0 10.0 4.5 0 Surfynol 104 Tergitol 15-S-30                      58-10 10 7.5 3.0 10.0 4.5 0 Neodol 25-3 ceteareth-55                           58-11 10 7.5 3.0 10.0 4.5 o Neodol 25-3 Tergitol 15-S-30                       58-12 10 7.5 3.0 10.0 4.5 0 Span 60 ceteareth-55                               58-13 10 7.5 3.0 10.0 4.5 0 Span 60 Tergitol 15-S-30                           58-14 10 7.5 3.0 10.0 4.5 0 oleth-2 ceteareth-55                               58-15 10 7.5 3.0 10.0 4.5 0 oleth-2 Tergitol 15-S-30                           58-16 10 7.5 3.0 10.0 4.5 0 Emid 6545 ceteareth-55                             58-17 10 7.5 3.0 10.0 4.5 0 Emid 6545 Tergitol 15-S-30                       __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 35 days after planting ABUTH and 33 days after planting ECHCF, and evaluation of herbicidal inhibition was done 17 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 58b.

                  TABLE 58b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0         0                                            250 35 40                                                                      350 50 63                                                                      450 60 43                                                                     Formulation C 150 63 63                                                         250 80 96                                                                      350 92 98                                                                      450 98 87                                                                     Formulation J 150 43 30                                                         250 75 85                                                                      350 82 98                                                                      450 96 95                                                                     58-01 150 65 53                                                                 250 85 70                                                                      350 90 87                                                                      450 98 73                                                                     58-02 150 63  5                                                                 250 78 53                                                                      350 88 80                                                                      450 97 87                                                                     58-03 150 75  0                                                                 250 87 22                                                                      350 88 72                                                                      450 97 17                                                                     58-04 150 84  0                                                                 250 90 10                                                                      350 95 70                                                                      450 98 60                                                                     58-05 150 77  0                                                                 250 83  3                                                                      350 93 30                                                                      450 95 10                                                                     58-06 150 72  0                                                                 250 83 47                                                                      350 94 60                                                                      450 98 20                                                                     58-07 150 75  0                                                                 250 77 40                                                                      350 96 47                                                                      450 96 50                                                                     58-08 150 87 40                                                                 250 97 82                                                                      350 99 83                                                                      450 100  77                                                                   58-09 150 82 10                                                                 250 82 40                                                                      350 96 67                                                                      450 97 67                                                                     58-10 150 82 13                                                                 250 94 83                                                                      350 99 85                                                                      450 99 83                                                                     58-11 150 73 17                                                                 250 83 60                                                                      350 88 73                                                                      450 96 63                                                                     58-12 150 80 20                                                                 250 93 85                                                                      350 96 82                                                                      450 96 82                                                                     58-13 150 78 20                                                                 250 83 50                                                                      350 92 90                                                                      450 92 85                                                                     58-14 150 80 30                                                                 250 97 85                                                                      350 99 99                                                                      450 97 96                                                                     58-15 150 82 30                                                                 250 87 75                                                                      350 99 92                                                                      450 99 93                                                                     58-16 150 82 53                                                                 250 96 82                                                                      350 96 97                                                                      450 87 82                                                                     58-17 150 72 20                                                                 250 80 63                                                                      350 92 75                                                                      450 95 87                                                                   ______________________________________                                    

Considerable variation was seen in herbicidal effectiveness of water-in-oil-in-water multiple emulsions of this Example, especially on ECHCF. Among the most efficacious were 58-08, 58-10, 58-12, 58-14 and 58-16. All of these contained a C₁₆₋₁₈ alkylether surfactant, ceteareth-55. When Tergitol 15-S-30, a C₁₂₋₁₅ secondary alkylether surfactant, replaced ceteareth-55, as in 58-09, 58-11, 58-13, 58-15 and 58-17, herbicidal effectiveness, at least on ECHCF, was in most cases markedly reduced.

Example 59

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 59a. Concentrate compositions 59-01 and 59-02 are water-in-oil-in-water multiple emulsions and were prepared by process (vi), using Span 80 as emulsifier #1. Concentrate compositions 59-03 to 59-12 and 59-14 to 59-17 are oil-in-water emulsions and were prepared by process (vii). Concentrate composition 59-13 is an aqueous solution concentrate and was prepared by process (viii), the component indicated below as "emulsifier #2" being the surfactant component.

                                      TABLE 59a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                           Butyl   Emulsifier                                                                          % in inner aq. Phase                                                                     Emulsifier                                    comp.                                                                              a.e.  stearate                                                                           Span 80                                                                            #2   Water                                                                              Glyphosate                                                                           #2                                            __________________________________________________________________________     59-01                                                                              10    18.0                                                                               3.0  5.0 12.2                                                                               20    Tween 20                                        59-02 10 7.5 3.0  5.0  5.3 20 Tween 20                                         59-03 10 1.0  10.0   Neodol 25-20                                              59-04 10 3.0  10.0   Neodol 25-20                                              59-05 10 1.0   5.0   Neodol 25-20                                              59-06 10 3.0   5.0   Neodol 25-20                                              59-07 15 1.0  10.0   Neodol 25-20                                              59-08 15 3.0  10.0   Neodol 25-20                                              59-09 15 1.0   5.0   Neodol 25-20                                              59-10 15 3.0   5.0   Neodol 25-20                                              59-11 20 1.0   5.0   Neodol 25-20                                              59-12 20 1.0  10.0   Neodol 25-20                                              59-13 10   10.0   Neodol 25-20                                                 59-14 10 7.5  10.0   Neodol 25-20                                              59-15 10 7.5  10.0   Neodol 25-20                                              59-16 10 7.5  10.0   steareth-20                                               59-17 10 7.5  10.0   oleth-20                                                __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and 19 days after planting ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, average for all replicates of each treatment, are shown in Table 59b.

                  TABLE 59b                                                        ______________________________________                                                     Glyphosate rate                                                                          % Inhibition                                             Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0        30                                            250 10 40                                                                      350 37 73                                                                      450 58 68                                                                     Formulation C 150 42 79                                                         250 77 98                                                                      350 99 97                                                                      450 97 93                                                                     Formulation J 150 43 67                                                         250 73 90                                                                      350 94 98                                                                      450 77 78                                                                     59-01 150 58 76                                                                 250 75 77                                                                      350 88 93                                                                      450 95 83                                                                     59-02 150 27 63                                                                 250 60 87                                                                      350 82 98                                                                      450 77 92                                                                     59-03 150 47 76                                                                 250 65 92                                                                      350 94 99                                                                      450 95 91                                                                     59-04 150 70 86                                                                 250 86 95                                                                      350 97 98                                                                      450 99 90                                                                     59-05 150 42 80                                                                 250 72 90                                                                      350 90 93                                                                      450 99 96                                                                     59-06 150 48 57                                                                 250 78 92                                                                      350 94 99                                                                      450 96 92                                                                     59-07 150 78 95                                                                 250 96 96                                                                      350 98 98                                                                      450 100  97                                                                   59-08 150 88 96                                                                 250 98 98                                                                      350 100  99                                                                    450 100  99                                                                   59-09 150 82 93                                                                 250 94 96                                                                      350 99 97                                                                      450 99 93                                                                     59-10 150 72 83                                                                 250 97 93                                                                      350 99 100                                                                     450 100  98                                                                   59-11 150 87 83                                                                 250 98 97                                                                      350 100  99                                                                    450 100  99                                                                   59-12 150 93 99                                                                 250 99 99                                                                      350 99 97                                                                      450 100  99                                                                   59-13 150 70 90                                                                 250 91 88                                                                      350 97 94                                                                      450 99 86                                                                     59-14 150 67 76                                                                 250 93 80                                                                      350 98 95                                                                      450 95 78                                                                     59-15 150 68 65                                                                 250 90 87                                                                      350 97 80                                                                      450 98 93                                                                     59-16 150 83 73                                                                 250 90 93                                                                      350 99 100                                                                     450 100  100                                                                  59-17 150 80 66                                                                 250 98 77                                                                      350 99 83                                                                      450 100  85                                                                 ______________________________________                                    

Very high herbicidal activity was evident in compositions 59-13 to 59-17, which have a very high ratio of surfactant to glyphosate a.e. of 1:1. Activity was too high to clearly distinguish among these compositions, but 59-16 and 59-17, containing steareth-20 and oleth-20 respectively, exbited greater effectiveness on ABUTH at the lowest glyphosate rate than 59-14 and 59-15, containing Neodol 25-20 and Neodol 25-12 respectively.

Example 60

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 60a. Concentrate compositions 60-01 and 60-02 are water-in-oil-in-water multiple emulsions and were prepared by process (vi), using Span 80 as emulsifier #1. Concentrate compositions 60-03 to 60-12 and 60-14 to 60-17 are oil-in-water emulsions and were prepared by process (vii). Concentrate composition 60-13 is an aqueous solution concentrate and was prepared by process (viii), the component indicated below as "emulsifier #2" being the surfactant component.

                                      TABLE 60a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                           Butyl   Emulsifier                                                                          % in inner aq. phase                                                                    Emulsifier                                     comp.                                                                              a.e.  stearate                                                                           Span 80                                                                            #2   Water                                                                              Glyphosate                                                                           #2                                            __________________________________________________________________________     60-01                                                                              10    18.0                                                                               3.0  5.0 12.2                                                                               20    Tween 20                                        60-02 10 7.5 3.0  5.0  5.3 20 Tween 20                                         60-03 10 1.0  10.0   Tween 80                                                  60-04 10 3.0  10.0   Tween 80                                                  60-05 10 1.0   5.0   Tween 80                                                  60-06 10 3.0   5.0   Tween 80                                                  60-07 15 1.0  10.0   Tween 80                                                  60-08 15 3.0  10.0   Tween 80                                                  60-09 15 1.0   5.0   Tween 80                                                  60-10 15 3.0   5.0   Tween 80                                                  60-11 20 1.0   5.0   Tween 80                                                  60-12 20 1.0  10.0   Tween 80                                                  60-13 10   10.0   Tween 80                                                     60-14 10 7.5  10.0   Tween 80                                                  60-15 10 7.5  10.0   Neodol 25-20                                              60-16 10 7.5  10.0   steareth-20                                               60-17 10 7.5  10.0   oleth-20                                                __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and 19 days after planting ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 60b.

                  TABLE 60b                                                        ______________________________________                                         Composition                                                                               Glyphosate rate                                                                             % Inhibition                                           applied    g a.e./ha    ABUTH    ECHCF                                         ______________________________________                                         Formulation B                                                                             150           0        0                                               250  3 10                                                                      350 17 20                                                                      450 20 30                                                                     Formulation C 150 70 33                                                         250 80 70                                                                      350 85 80                                                                      450 97 77                                                                     Formulation J 150  7 20                                                         250 70 80                                                                      350 78 80                                                                      450 83 80                                                                     60-01 150 40  7                                                                 250 48 20                                                                      350 73 23                                                                      450 75 30                                                                     60-02 150  3  0                                                                 250 10 17                                                                      350 47 23                                                                      450 50 30                                                                     60-03 150  0  2                                                                 250 33 13                                                                      350 63 40                                                                      450 68 43                                                                     60-04 150 17  7                                                                 250 43 20                                                                      350 78 63                                                                      450 78 63                                                                     60-05 150 10  3                                                                 250 20 13                                                                      350 58 40                                                                      450 75 40                                                                     60-06 150  3  0                                                                 250 27 20                                                                      350 60 23                                                                      450 72 23                                                                     60-07 150 32 10                                                                 250 68 20                                                                      350 75 50                                                                      450 86 60                                                                     60-08 150 27 20                                                                 250 68 30                                                                      350 82 40                                                                      450 90 73                                                                     60-09 150 43 10                                                                 250 60 33                                                                      350 72 63                                                                      450 75 73                                                                     60-10 150 33 10                                                                 250 62 30                                                                      350 77 60                                                                      450 83 70                                                                     60-11 150 48 13                                                                 250 72 63                                                                      350 83 80                                                                      450 87 80                                                                     60-12 150 23 13                                                                 250 60 50                                                                      350 75 80                                                                      450 86 78                                                                     60-13 150 32 13                                                                 250 47 40                                                                      350 75 50                                                                      450 78 70                                                                     60-14 150 27 20                                                                 250 75 53                                                                      350 82 70                                                                      450 92 67                                                                     60-15 150 70 20                                                                 250 78 30                                                                      350 92 80                                                                      450 93 80                                                                     60-16 150 68 40                                                                 250 73 30                                                                      350 93 80                                                                      450 93 77                                                                     60-17 150 73 20                                                                 250 85 30                                                                      350 93 60                                                                      450 95 63                                                                   ______________________________________                                    

Compositions 60-16 and 60-17, containing steareth-20 and oleth-20 respectively, exhibited very high herbicidal activity on ABUTH. At the very high surfactant to glyphosate a.e. ratio (1:1) of these compositions, no difference was evident between these compositions and an otherwise similar composition (60-15) containing Neodol 25-20 in place of steareth-20 or oleth-20.

Example 61

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 61a. All are oil-in-water emulsions and were prepared by process (vii).

                  TABLE 61a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl          Type of                                        composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         61-01    163       1.00    10.0   Tween 80                                       61-02 163 1.00 10.0 Neodol 25-12                                               61-03 163 1.00 10.0 Neodol 25-20                                               61-04 163 1.00 10.0 steareth-20                                                61-05 163 1.00 10.0 oleth-20                                                   61-06 163 1.00 10.0 Tergitol 15-S-40                                           61-07 163 1.00 10.0 Tergitol 15-S-15                                           61-08 163 1.00 10.0 Tergitol 15-S-20                                           61-09 163 0.50 10.0 Tergitol 15-S-40                                           61-10 163 0.50 10.0 Tergitol 15-S-15                                           61-11 163 0.50 10.0 Tergitol 15-S-20                                           61-12 163 0.50 5.0 Tergitol 15-S-40                                            61-13 163 0.50 5.0 Tergitol 15-S-15                                            61-14 163 0.50 5.0 Tergitol 15-S-20                                            61-15 163 0.25 10.0 Tergitol 15-S-40                                         ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 61b.

                  TABLE 61b                                                        ______________________________________                                         Concentrate                                                                               Glyphosate rate                                                                             % Inhibition                                           composition                                                                               g a.e./ha    ABUTH    ECHCF                                         ______________________________________                                         Formulation B                                                                             150           2       20                                               250  2 30                                                                      350  5 53                                                                      450 45 75                                                                     Formulation C 150 45 63                                                         250 77 93                                                                      350 83 99                                                                      450 93 100                                                                    Formulation J 150 15 40                                                         250 70 73                                                                      350 78 98                                                                      450 92 99                                                                     61-01 150 42 50                                                                 250 72 89                                                                      350 80 96                                                                      450 93 98                                                                     61-02 150 45 80                                                                 250 72 83                                                                      350 85 91                                                                      450 97 98                                                                     61-03 150 60 80                                                                 250 75 87                                                                      350 82 96                                                                      450 86 99                                                                     61-04 150 65 60                                                                 250 82 70                                                                      350 93 80                                                                      450 98 87                                                                     61-05 150 72 60                                                                 250 83 87                                                                      350 95 93                                                                      450 98 97                                                                     61-06 150 50 45                                                                 250 68 70                                                                      350 77 85                                                                      450 83 90                                                                     61-07 150 25 40                                                                 250 65 50                                                                      350 80 77                                                                      450 83 80                                                                     61-08 150 37 33                                                                 250 72 80                                                                      350 77 87                                                                      450 80 90                                                                     61-09 150 32 47                                                                 250 65 73                                                                      350 77 75                                                                      450 80 94                                                                     61-10 150 17 30                                                                 250 65 70                                                                      350 75 70                                                                      450 78 89                                                                     61-11 150 35 33                                                                 250 68 68                                                                      350 77 77                                                                      450 92 75                                                                     61-12 150 13 35                                                                 250 57 40                                                                      350 75 57                                                                      450 77 83                                                                     61-13 150 35 40                                                                 250 63 43                                                                      350 77 77                                                                      450 83 75                                                                     61-14 150 30 25                                                                 250 67 53                                                                      350 78 85                                                                      450 83 77                                                                     61-15 150 13 37                                                                 250 65 50                                                                      350 77 57                                                                      450 87 82                                                                   ______________________________________                                    

At a surfactant to glyphosate a.e. weight/weight ratio of about 1:1.5, compositions containing steareth-20 or oleth-20 (61-04 and 61-05 respectively) exhibited herbicidal effectiveness on ABUTH similar to one containing Neodol 25-20 (61-03).

Example 62

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 62a. All are oil-in-water emulsions and were prepared by process (vii).

                  TABLE 62a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl          Type of                                        composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         62-01    163       1.0     10.0   Tween 80                                       62-02 163 1.0 10.0 Neodol 25-12                                                62-03 163 1.0 10.0 Neodol 25-20                                                62-04 163 1.0 10.0 steareth-20                                                 62-05 163 1.0 10.0 oleth-20                                                    62-06 163 1.0 10.0 Tergitol 15-S-40                                            62-06 163 1.0 10.0 Tergitol 15-S-15                                            62-08 163 1.0 10.0 Tergitol 15-S-20                                            62-09 163 0.5 10.0 Tergitol 15-S-40                                            62-10 163 0.3 10.0 Tergitol 15-S-15                                            62-11 163 0.3 10.0 Tergitol 15-S-20                                            62-12 163 0.3 10.0 Tergitol 15-S-40                                            62-13 163 0.3 5.0 Tergitol 15-S-15                                             62-14 163 0.3 5.0 Tergitol 15-S-20                                             62-15 163 0.3 5.0 Tergitol 15-S-40                                           ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 21 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 62b.

                  TABLE 62b                                                        ______________________________________                                         Concentrate                                                                               Glyphosate rate                                                                             % Inhibition                                           composition                                                                               g a.e./ha    ABUTH    ECHCF                                         ______________________________________                                         Formulation B                                                                             150          0        23                                               250 0 40                                                                       350 5 53                                                                       450 13 57                                                                     Formulation C 150 0 47                                                          250 28 87                                                                      350 72 98                                                                      450 97 97                                                                     Formulation J 150 5 40                                                          250 20 63                                                                      350 67 93                                                                      450 82 92                                                                     62-01 150 2 40                                                                  250 30 50                                                                      350 50 70                                                                      450 57 85                                                                     62-02 150 10 50                                                                 250 33 50                                                                      350 75 72                                                                      450 75 88                                                                     62-03 150 17 53                                                                 250 60 60                                                                      350 70 92                                                                      450 78 94                                                                     62-04 150 57 45                                                                 250 70 70                                                                      350 82 93                                                                      450 83 95                                                                     62-05 150 47 45                                                                 250 70 80                                                                      350 80 88                                                                      450 88 92                                                                     62-06 150 2 42                                                                  250 20 60                                                                      350 35 75                                                                      450 58 89                                                                     62-07 150 0 42                                                                  250 30 68                                                                      350 40 75                                                                      450 77 82                                                                     62-08 150 2 40                                                                  250 25 60                                                                      350 50 83                                                                      450 75 86                                                                     62-09 150 2 43                                                                  250 27 83                                                                      350 40 73                                                                      450 70 78                                                                     62-10 150 2 42                                                                  250 32 47                                                                      350 43 63                                                                      450 70 82                                                                     62-11 150 0 30                                                                  250 25 53                                                                      350 35 75                                                                      450 70 75                                                                     62-12 150 2 40                                                                  250 13 57                                                                      350 25 75                                                                      450 40 83                                                                     62-13 150 5 42                                                                  250 23 62                                                                      350 38 63                                                                      450 67 60                                                                     62-14 150 2 33                                                                  250 13 48                                                                      350 30 53                                                                      450 70 88                                                                     62-15 150 2 33                                                                  250 18 48                                                                      350 30 75                                                                      450 43 65                                                                   ______________________________________                                    

In this test, herbicidal effectiveness overall was lower than in the previous Example, particularly on ABUTH. In these circumstances, at a surfactant to glyphosate a.e. weight/weight ratio of about 1:1.5, compositions containing steareth-20 or oleth-20 (62-04 and 62-05 respectively) exhibited greater herbicidal effectiveness on both ABUTH and ECHCF than one containing Neodol 25-20 (62-03).

Example 63

Aqueous concentrate compositions were prepared containing glyphosate ammonium or IPA salt and excipient ingredients as shown in Table 63a. Concentrate composition 63-01 is a water-in-oil-in-water multiple emulsion and was prepared by process (vi), using Span 80 as emulsifier #1. Concentrate compositions 63-02 to 63-11 and 63-17 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 63-12 to 63-16 are aqueous solution concentrates and were prepared by process (viii), the component indicated below as "emulsifier #2" being the surfactant component.

                                      TABLE 63a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                           Butyl   Emulsifier                                                                          % in inner aq. phase                                                                     Emulsifier                                                                            Glyphosate                             comp.                                                                              a.e.  stearate                                                                           Span 80                                                                            #2   Water                                                                              Glyphosate                                                                           #2     salt                                   __________________________________________________________________________     63-01                                                                              10    18.0                                                                               3.0  5.0 9.0 20    Tween 20                                                                              IPA                                      63-02 15 1.0  10.0   Tween 80 IPA                                              63-03 15 1.0  10.0   Neodol 25-12 IPA                                          63-04 15 1.0  10.0   Neodol 25-20 IPA                                          63-05 15 1.0  10.0   steareth-20 IPA                                           63-06 15 1.0  10.0   oleth-20 IPA                                              63-07 15 1.0  10.0   Tween 80 ammonium                                         63-08 15 1.0  10.0   Neodol 25-12 ammonium                                     63-09 15 1.0  10.0   Neodol 25-20 ammonium                                     63-10 15 1.0  10.0   steareth-20 ammonium                                      63-11 15 1.0  10.0   oleth-20 ammonium                                         63-12 15   10.0   Tween 80 IPA                                                 63-13 15   10.0   Neodol 25-12 IPA                                             63-14 15   10.0   Neodol 25-20 IPA                                             63-15 15   10.0   steareth-20 IPA                                              63-16 15   10.0   oleth-20 IPA                                                 63-17 15 1.0  10.0   Emerest 2661 IPA                                        __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 63b.

                  TABLE 63b                                                        ______________________________________                                         Concentrate                                                                               Glyphosate rate                                                                             % Inhibition                                           composition                                                                               g a.e./ha    ABUTH    ECHCF                                         ______________________________________                                         Formulation B                                                                             150          2         5                                               250 3 25                                                                       350 28 30                                                                      450 53 50                                                                     Formulation C 150 5 25                                                          250 60 50                                                                      350 85 83                                                                      450 88 88                                                                     Formulation J 150 2 10                                                          250 70 40                                                                      350 82 53                                                                      450 87 83                                                                     63-01 150 23 20                                                                 250 72 30                                                                      350 80 80                                                                      450 85 69                                                                     63-02 150 5 18                                                                  250 72 38                                                                      350 82 63                                                                      450 85 83                                                                     63-03 150 25 20                                                                 250 70 57                                                                      350 85 68                                                                      450 90 83                                                                     63-04 150 25 27                                                                 250 77 67                                                                      350 85 62                                                                      450 88 70                                                                     63-05 150 60 25                                                                 250 82 62                                                                      350 87 73                                                                      450 85 80                                                                     63-06 150 50 32                                                                 250 78 78                                                                      350 91 91                                                                      450 98 98                                                                     63-07 150 5 25                                                                  250 55 77                                                                      350 77 86                                                                      450 83 99                                                                     63-08 150 0 13                                                                  250 58 78                                                                      350 80 85                                                                      450 85 87                                                                     63-09 150 7 25                                                                  250 57 72                                                                      350 77 83                                                                      450 91 92                                                                     63-10 150 50 25                                                                 250 80 55                                                                      350 86 87                                                                      450 92 82                                                                     63-11 150 53 30                                                                 250 78 80                                                                      350 87 89                                                                      450 95 98                                                                     63-12 150 0 25                                                                  250 50 77                                                                      350 77 90                                                                      450 83 94                                                                     63-13 150 2 30                                                                  250 55 75                                                                      350 72 92                                                                      450 85 80                                                                     63-14 150 12 30                                                                 250 75 78                                                                      350 84 90                                                                      450 96 94                                                                     63-15 150 55 35                                                                 250 78 80                                                                      350 80 94                                                                      450 86 98                                                                     63-16 150 50 35                                                                 250 73 63                                                                      350 84 83                                                                      450 89 95                                                                     63-17 150 0 10                                                                  250 10 53                                                                      350 53 83                                                                      450 62 87                                                                   ______________________________________                                    

Compositions containing steareth-20 or oleth-20 (63-05, 63-06, 63-10, 63-11, 63-15, 63-16) generally exhibited superior herbicidal effectiveness to counterparts containing Neodol 25-20 (63-04, 63-09, 63-14) at least on ABUTH. The presence of a small amount of butyl stearate tended to enhance effectiveness on ABUTH (compare 63-05 and 63-06 with 63-15 and 63-16).

Example 64

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 64a. Concentrate composition 64-01 is a water-in-oil-in-water multiple emulsion and was prepared by process (vi), using Span 80 as emulsifier # 1. Concentrate compositions 64-02 to 64-08, 64-14, 64-16 and 64-17 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 64-09 to 64-13 and 64-15 are aqueous solution concentrates and were prepared by process (viii), the component indicated below as "emulsifier #2" being the surfactant component.

                                      TABLE 64a                                    __________________________________________________________________________     % w/w                                                                          Conc.                                                                              Glyphosate                                                                           Butyl   Emulsifier                                                                          % in inner aq. phase                                                                     Emulsifier                                    comp.                                                                              a.e.  stearate                                                                           Span 80                                                                            #2   Water                                                                              Glyphosate                                                                           #2                                            __________________________________________________________________________     64-01                                                                              10    18.0                                                                               3.0  2.5 9.0 20    Tween 20                                        64-02 15 1.0  10.0   Emerest 2661                                              64-03 15 1.0  10.0   Tween 80                                                  64-04 15 1.0  10.0   oleth-20                                                  64-05 15 1.0  10.0   Neodol 25-20                                              64-06 15 1.0  10.0   ceteareth-27                                              64-07 15 1.0  10.0   ceteareth-55                                              64-08 15 1.0  10.0   Genapol UD-110                                            64-09 15   10.0   ceteareth-27                                                 64-10 15   10.0   ceteareth-55                                                 64-11 15   10.0   Genapol UD-110                                               64-12 15   10.0   oleth-20                                                     64-13 10   10.0   oleth-20                                                     64-14 10 1.0  10.0   oleth-20                                                  64-15 20   10.0   oleth-20                                                     64-16 15 0.5   5.0   oleth-20                                                  64-17 15 0.5  10.0   oleth-20                                                __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 64b.

                  TABLE 64b                                                        ______________________________________                                         Concentrate                                                                               Glyphosate rate                                                                             % Inhibition                                           composition                                                                               g a.e./ha    ABUTH    ECHCF                                         ______________________________________                                         Formulation B                                                                             150           0        0                                               250  8 20                                                                      350 27 40                                                                      450 62 50                                                                     Formulation C 150 27 50                                                         250 75 70                                                                      350 92 80                                                                      450 97 92                                                                     Formulation J 150 23 30                                                         250 72 50                                                                      350 94 63                                                                      450 95 80                                                                     64-01 150 22 30                                                                 250 60 40                                                                      350 83 57                                                                      450 90 67                                                                     64-02 150 12 33                                                                 250 45 50                                                                      350 73 63                                                                      450 83 83                                                                     64-03 150 27 43                                                                 250 68 50                                                                      350 80 63                                                                      450 87 87                                                                     64-04 150 68 47                                                                 250 95 73                                                                      350 99 78                                                                      450 95 90                                                                     64-05 150 50 50                                                                 250 77 77                                                                      350 90 83                                                                      450 98 83                                                                     64-06 150 78 67                                                                 250 93 82                                                                      350 97 87                                                                      450 99 97                                                                     64-07 150 87 57                                                                 250 96 73                                                                      350 99 85                                                                      450 99 97                                                                     64-08 150 42 30                                                                 250 73 53                                                                      350 82 85                                                                      450 95 89                                                                     64-09 150 67 40                                                                 250 95 73                                                                      350 99 95                                                                      450 99 98                                                                     64-10 150 85 60                                                                 250 96 68                                                                      350 96 91                                                                      450 100  88                                                                   64-11 150 13 10                                                                 250 67 50                                                                      350 78 60                                                                      450 88 73                                                                     64-12 150 72 43                                                                 250 97 68                                                                      350 98 83                                                                      450 99 93                                                                     64-13 150 73 57                                                                 250 88 70                                                                      350 98 87                                                                      450 99 96                                                                     64-14 150 80 50                                                                 250 96 70                                                                      350 99 85                                                                      450 98 88                                                                     64-15 150 70 43                                                                 250 96 53                                                                      350 97 82                                                                      450 99 89                                                                     64-16 150 62 53                                                                 250 88 72                                                                      350 99 81                                                                      450 99 91                                                                     64-17 150 72 58                                                                 250 95 68                                                                      350 100  89                                                                    450 100  93                                                                 ______________________________________                                    

The greatest herbicidal effectiveness in this test was exhibited by compositions containing a C₁₆₋₁₈ alkylether surfactant (oleth-20, ceteareth-27 or ceteareth-55).

Example 65

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 65a. All are oil-in-water emulsions and were prepared by process (vii).

                  TABLE 65a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl          Type of                                        composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         65-01    163       1.00    10.0   Tween 80                                       65-02 163 1.00 10.0 Emerest 2661                                               65-03 326 1.00 10.0 Genapol UD-110                                             65-04 326 0.50 10.0 Genapol UD-110                                             65-05 326 0.25 10.0 Genapol UD-110                                             65-06 163 0.25 10.0 Genapol UD-110                                             65-07 163 1.00 10.0 Genapol UD-110                                             65-08 163 1.00 10.0 Neodol 1-9                                                 65-09 163 1.00 10.0 Neodol 1-12                                                65-10 163 1.00 10.0 Neodol 25-20                                               65-11 163 1.00 10.0 Neodol 25-12                                               65-12 163 1.00 10.0 Neodox 25-11                                               65-13 163 1.00 10.0 laureth-23                                                 65-14 163 1.00 10.0 ceteth-20                                                  65-15 163 1.00 10.0 steareth-20                                                65-16 163 1.00 10.0 oleth-20                                                 ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 234 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 65b.

                  TABLE 65b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         0         0                                             250 25 22                                                                      350 60 40                                                                      450 65 52                                                                     Formulation C 150 43 52                                                         250 72 83                                                                      350 87 98                                                                      450 97 95                                                                     Formulation J 150 50 43                                                         250 75 91                                                                      350 86 96                                                                      450 95 97                                                                     65-01 150 50 30                                                                 250 75 75                                                                      350 85 87                                                                      450 90 92                                                                     65-02 150 35 47                                                                 250 58 77                                                                      350 75 85                                                                      450 80 96                                                                     65-03 150 33 32                                                                 250 57 53                                                                      350 75 78                                                                      450 84 94                                                                     65-04 150 20 25                                                                 250 55 68                                                                      350 78 91                                                                      450 82 97                                                                     65-05 150 37 12                                                                 250 58 42                                                                      350 81 70                                                                      450 86 73                                                                     65-06 150 50 8                                                                  250 65 40                                                                      350 81 65                                                                      450 92 85                                                                     65-07 150 50 30                                                                 250 63 48                                                                      350 84 68                                                                      450 98 84                                                                     65-08 150 43 35                                                                 250 52 65                                                                      350 73 85                                                                      450 84 85                                                                     65-09 150 55 40                                                                 250 68 58                                                                      350 79 65                                                                      450 97 73                                                                     65-10 150 69 40                                                                 250 81 68                                                                      350 94 92                                                                      450 99 96                                                                     65-11 150 58 50                                                                 250 84 60                                                                      350 90 83                                                                      450 94 93                                                                     65-12 150 50 40                                                                 250 57 67                                                                      350 65 84                                                                      450 75 98                                                                     65-13 150 57 53                                                                 250 78 73                                                                      350 89 97                                                                      450 98 97                                                                     65-14 150 68 67                                                                 250 85 73                                                                      350 97 98                                                                      450 100 97                                                                    65-15 150 72 50                                                                 250 88 89                                                                      350 89 98                                                                      450 99 97                                                                     65-16 150 65 53                                                                 250 87 72                                                                      350 97 85                                                                      450 100 95                                                                  ______________________________________                                    

Activity overall in this test was very high, and differences among compositions in herbicidal effectiveness are difficult to discern clearly.

Example 66

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 66a. All are oil-in-water emulsions and were prepared by process (vii). The pH of all compositions was approximately 5.

                  TABLE 66a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl           Type of                                       composition g a.e./l Stearate Surfactant surfactant                          ______________________________________                                         66-01    163       1.00     10.0   Tween 80                                      66-02 163 1.00 10.0 Emerest 2661                                               66-03 163 1.00 10.0 Neodol 25-20                                               66-04 163 1.00 10.0 oleth-20                                                   66-05 163 0.50 5.0 oleth-20                                                    66-06 163 0.25 2.5 oleth-20                                                    66-07 163 0.50 2.5 oleth-20                                                    66-08 163 0.50 1.0 oleth-20                                                    66-09 163 0.25 5.0 oleth-20                                                    66-10 326 1.00 10.0 Neodol 1-12                                                66-11 326 0.50 10.0 Neodol 1-12                                                66-12 326 0.25 10.0 Neodol 1-12                                                66-13 326 1.00 5.0 Neodol 1-12                                                 66-14 326 0.50 5.0 Neodol 1-12                                                 66-15 326 0.25 5.0 Neodol 1-12                                                 66-16 326 0.10 5.0 Neodol 1-12                                               ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 15 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 66b.

                  TABLE 66b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         7         50                                            250 45 60                                                                      350 73 73                                                                      450 80 78                                                                     Formulation C 150 75 77                                                         250 87 100                                                                     350 96 99                                                                      450 99 97                                                                     Formulation J 150 72 77                                                         250 83 89                                                                      350 97 99                                                                      450 97 98                                                                     66-01 150 60 75                                                                 250 80 85                                                                      350 93 97                                                                      450 98 98                                                                     66-02 150 57 75                                                                 250 70 83                                                                      350 87 83                                                                      450 90 94                                                                     66-03 150 77 80                                                                 250 87 92                                                                      350 97 87                                                                      450 99 98                                                                     66-04 150 80 89                                                                 250 93 92                                                                      350 99 99                                                                      450 100 99                                                                    66-05 150 83 83                                                                 250 92 93                                                                      350 97 90                                                                      450 100 93                                                                    66-06 150 77 77                                                                 250 80 91                                                                      350 90 99                                                                      450 98 99                                                                     66-07 150 77 83                                                                 250 82 89                                                                      350 90 91                                                                      450 97 98                                                                     66-08 150 47 82                                                                 250 73 82                                                                      350 80 97                                                                      450 92 91                                                                     66-09 150 73 78                                                                 250 87 88                                                                      350 97 94                                                                      450 99 99                                                                     66-10 150 52 67                                                                 250 70 80                                                                      350 93 88                                                                      450 93 94                                                                     66-11 150 40 68                                                                 250 72 85                                                                      350 87 96                                                                      450 93 96                                                                     66-12 150 37 60                                                                 250 68 83                                                                      350 85 85                                                                      450 93 75                                                                     66-13 150 28 63                                                                 250 53 80                                                                      350 85 97                                                                      450 88 97                                                                     66-14 150 37 63                                                                 250 58 73                                                                      350 83 96                                                                      450 90 91                                                                     66-15 150 30 70                                                                 250 47 83                                                                      350 82 89                                                                      450 87 89                                                                     66-16 150 40 53                                                                 250 53 82                                                                      350 80 80                                                                      450 88 77                                                                   ______________________________________                                    

Composition 66-04, containing 1% butyl stearate and 10% oleth-20 (surfactant to glyphosate a.e. weight/weight ratio about 1:1.5), exhibited marginally greater herbicidal effectiveness than composition 66-03, containing 1% butyl stearate and 10% Neodol 25-20. At this very high surfactant to glyphosate ratio, however, both performed extremely well. Surprisingly, when the butyl stearate and oleth-20 concentrations were significantly lowered, this high level of performance was maintained to a remarkable degree. Even when butyl stearate was reduced to 0.25% and oleth-20 to 2.5% (surfactant to glyphosate a.e. ratio about 1:6), as in composition 66-06, herbicidal effectiveness was still similar to that obtained with commercial standard Formulations C and J.

Example 67

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 67a. Concentrate compositions 67-01 to 67-08 and 67-11 to 67-16 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 67-09 and 67-10 are aqueous solution concentrates and were prepared by process (viii). The pH of all compositions was approximately 5.

                  TABLE 67a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl           Type of                                       composition a.e. Stearate Surfactant surfactant                              ______________________________________                                         67-01    15.0      0.25     5.0    Emerest 2661                                  67-02 15.0 0.25 5.0 Tween 80                                                   67-03 15.0 0.25 5.0 Neodol 25-20                                               67-04 15.0 0.25 5.0 laureth-23                                                 67-05 15.0 0.25 5.0 ceteth-20                                                  67-06 15.0 0.25 2.5 Tween 80                                                   67-07 15.0 0.10 1.0 Tween 80                                                   67-08 15.0 1.00 10.0 Tween 80                                                  67-09 15.0  5.0 laureth-23                                                     67-10 15.0  5.0 ceteth-20                                                      67-11 15.0 1.00 10.0 Neodol 25-20                                              67-12 15.0 1.00 10.0 oleth-20                                                  67-13 15.0 0.50 5.0 oleth-20                                                   67-14 15.0 0.25 5.0 oleth-20                                                   67-15 15.0 0.25 2.5 oleth-20                                                   67-16 15.0 0.25 5.0 Genapol UD-110                                           ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 12 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 67b.

                  TABLE 67b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         2         10                                            250 5 20                                                                       350 43 30                                                                      450 58 43                                                                     Formulation C 150 68 50                                                         250 92 79                                                                      350 96 90                                                                      450 98 85                                                                     Formulation J 150 57 43                                                         250 90 63                                                                      350 95 80                                                                      450 95 95                                                                     67-01 150 7 33                                                                  250 50 43                                                                      350 77 53                                                                      450 80 93                                                                     67-02 150 17 50                                                                 250 72 70                                                                      350 80 80                                                                      450 80 93                                                                     67-03 150 43 40                                                                 250 75 68                                                                      350 87 75                                                                      450 96 95                                                                     67-04 150 33 47                                                                 250 73 63                                                                      350 80 77                                                                      450 90 93                                                                     67-05 150 73 37                                                                 250 92 57                                                                      350 95 88                                                                      450 95 73                                                                     67-06 150 25 35                                                                 250 68 47                                                                      350 80 92                                                                      450 88 85                                                                     67-07 150 3 30                                                                  250 57 40                                                                      350 77 53                                                                      450 80 67                                                                     67-08 150 53 43                                                                 250 77 62                                                                      350 80 88                                                                      450 93 80                                                                     67-09 150 32 60                                                                 250 77 53                                                                      350 93 73                                                                      450 97 93                                                                     67-10 150 75 35                                                                 250 92 77                                                                      350 96 77                                                                      450 97 93                                                                     67-11 150 75 53                                                                 250 90 78                                                                      350 95 89                                                                      450 98 97                                                                     67-12 150 80 43                                                                 250 95 73                                                                      350 96 92                                                                      450 98 89                                                                     67-13 150 75 53                                                                 250 92 97                                                                      350 97 99                                                                      450 96 93                                                                     67-14 150 78 70                                                                 250 90 92                                                                      350 93 97                                                                      450 95 93                                                                     67-15 150 70 60                                                                 250 83 98                                                                      350 95 99                                                                      450 97 99                                                                     67-16 150 27 52                                                                 250 75 73                                                                      350 80 98                                                                      450 83 99                                                                   ______________________________________                                    

Extremely high herbicidal effectiveness was again observed with a composition (67-15) containing 15% glyphosate a.e. and just 2.5% oleth-20 together with 0.25% butyl stearate. A comparison of 15% glyphosate a.e. compositions containing 5% alkylether surfactant and 0.25% butyl stearate provided the following ranking of alkylethers in descending order of effectiveness: oleth-20 (67-14)>ceteth-20 (67-05)>Neodol 25-20 (67-03)=laureth-23 (67-04).

Example 68

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 68a. All are oil-in-water emulsions and were prepared by process (vii).

                  TABLE 68a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl           Type of                                       composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         68-01    163       0.50     5.0    oleth-20                                      68-02 163 0.25 5.0 oleth-20                                                    68-03 163 0.25 2.5 oleth-20                                                    68-04 163 1.00 10.0 oleth-20                                                   68-05 163 0.50 5.0 steareth-20                                                 68-06 163 0.25 5.0 steareth-20                                                 68-07 163 0.25 2.5 steareth-20                                                 68-08 163 1.00 10.0 steareth-20                                              ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 68b.

                  TABLE 68b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0        30                                            250 20 43                                                                      350 43 53                                                                      450 68 57                                                                     Formulation C 150 60 47                                                         250 75 53                                                                      350 87 80                                                                      450 87 78                                                                     Formulation J 150 42 43                                                         250 83 60                                                                      350 87 73                                                                      450 93 87                                                                     68-01 150 60 60                                                                 250 78 63                                                                      350 87 89                                                                      450 92 78                                                                     68-02 150 70 43                                                                 250 80 91                                                                      350 87 86                                                                      450 96 87                                                                     68-03 150 52 43                                                                 250 75 72                                                                      350 83 93                                                                      450 87 94                                                                     68-04 150 72 50                                                                 250 93 73                                                                      350 97 95                                                                      450 97 91                                                                     68-05 150 72 43                                                                 250 80 78                                                                      350 87 91                                                                      450 93 85                                                                     68-06 150 68 40                                                                 250 80 50                                                                      350 93 75                                                                      450 95 85                                                                     68-07 150 63 37                                                                 250 78 55                                                                      350 87 84                                                                      450 83 82                                                                     68-08 150 70 50                                                                 250 80 70                                                                      350 92 84                                                                      450 94 98                                                                   ______________________________________                                    

All compositions containing butyl stearate and either oleth-20 or steareth-20 showed a very high level of performance by comparison with commercial standard Formulations C and J.

Example 69

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 69a. All are oil-in-water emulsions and were prepared by process (vii).

                  TABLE 69a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl           Type of                                       composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         69-01    163       0.50     5.0    oleth-20                                      69-02 163 0.25 5.0 oleth-20                                                    69-03 163 0.25 2.5 oleth-20                                                    69-04 163 1.00 10.0 oleth-20                                                   69-05 163 0.50 5.0 steareth-20                                                 69-06 163 0.25 5.0 steareth-20                                                 69-07 163 0.25 2.5 steareth-20                                                 69-08 163 1.00 10.0 steareth-20                                              ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 69b.

                  TABLE 69b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          3        10                                            250 28 23                                                                      350 72 37                                                                      450 73 50                                                                     Formulation C 150 57 43                                                         250 87 62                                                                      350 93 83                                                                      450 99 95                                                                     Formulation J 150 27 47                                                         250 70 53                                                                      350 92 75                                                                      450 94 92                                                                     69-01 150 68 50                                                                 250 85 47                                                                      350 97 70                                                                      450 99 83                                                                     69-02 150 67 40                                                                 250 78 50                                                                      350 96 63                                                                      450 99 68                                                                     69-03 150 52 40                                                                 250 72 50                                                                      350 95 63                                                                      450 97 85                                                                     69-04 150 72 40                                                                 250 97 53                                                                      350 97 77                                                                      450 99 90                                                                     69-05 150 75 40                                                                 250 missing 53                                                                 350 88 53                                                                      450 96 78                                                                     69-06 150 98 40                                                                 250 93 50                                                                      350 97 68                                                                      450 97 82                                                                     69-07 150 73 40                                                                 250 92 50                                                                      350 98 63                                                                      450 98 80                                                                     69-08 150 77 43                                                                 250 93 57                                                                      350 97 77                                                                      450 98 88                                                                   ______________________________________                                    

All compositions containing butyl stearate and either oleth-20 or steareth-20 showed a very high level of performance by comparison with commercial standard Formulations C and J.

Example 70

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 70a. All contain colloidal particulates and were prepared by process (ix).

All compositions of this example showed acceptable storage stability. The compositions containing oleth-20 were not acceptably storage-stable in the absence of the colloidal particulate.

                  TABLE 70a                                                        ______________________________________                                                     % w/w                                                              Concentrate                                                                            Glyphosate                                                                               Butyl                Type of                                   composition g a.e./l stearate Oleth-20 Aerosil Aerosil                       ______________________________________                                         70-01   488               3.0    0.4   OX-50                                     70-02 488  3.0 0.8 OX-50                                                       70-03 488  3.0 1.5 OX-50                                                       70-04 488   0.4 OX-50                                                          70-05 488   0.8 OX-50                                                          70-06 488   1.5 OX-50                                                          70-07 488  3.0 0.4 MOX-80                                                      70-08 488  3.0 0.8 MOX-80                                                      70-09 488  3.0 1.5 MOX-80                                                      70-10 488   0.4 MOX-80                                                         70-11 488   0.8 MOX-80                                                         70-12 488   1.5 MOX-80                                                         70-13 488  3.0 0.4 MOX-170                                                     70-14 488  3.0 0.8 MOX-170                                                     70-15 488  3.0 1.5 MOX-170                                                     70-16 488   0.4 MOX-170                                                        70-17 488   0.8 MOX-170                                                        70-18 488   1.5 MOX-170                                                        70-19 488 3.0 3.0 1.5 MOX-80                                                 ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 70b.

                  TABLE 70b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0        27                                            250 17 37                                                                      350 47 57                                                                      450 60 60                                                                     Formulation J 150 57 50                                                         250 82 87                                                                      350 95 99                                                                      450 98 99                                                                     70-01 150 37 60                                                                 250 73 70                                                                      350 96 97                                                                      450 96 99                                                                     70-02 150 43 50                                                                 250 73 63                                                                      350 93 96                                                                      450 98 99                                                                     70-03 150 53 60                                                                 250 83 87                                                                      350 87 97                                                                      450 98 98                                                                     70-04 150 45 40                                                                 250 57 60                                                                      350 78 95                                                                      450 94 100                                                                    70-05 150 47 50                                                                 250 60 82                                                                      350 92 96                                                                      450 95 99                                                                     70-06 150 38 53                                                                 250 68 96                                                                      350 82 99                                                                      450 83 95                                                                     70-07 150 50 57                                                                 250 87 88                                                                      350 91 99                                                                      450 98 98                                                                     70-08 150 53 50                                                                 250 88 85                                                                      350 96 97                                                                      450 97 100                                                                    70-09 150 40 30                                                                 250 37 47                                                                      350 57 80                                                                      450 77 94                                                                     70-10 150 47 50                                                                 250 70 95                                                                      350 75 99                                                                      450 77 98                                                                     70-11 150 27 60                                                                 250 72 85                                                                      350 82 98                                                                      450 75 99                                                                     70-12 150 37 57                                                                 250 73 86                                                                      350 80 99                                                                      450 85 100                                                                    70-13 150 45 53                                                                 250 85 94                                                                      350 95 100                                                                     450 98 99                                                                     70-14 150 50 50                                                                 250 78 83                                                                      350 94 98                                                                      450 98 99                                                                     70-15 150 53 67                                                                 250 75 88                                                                      350 93 97                                                                      450 96 99                                                                     70-16 150 42 50                                                                 250 47 96                                                                      350 70 98                                                                      450 90 99                                                                     70-17 150 27 83                                                                 250 57 98                                                                      350 87 99                                                                      450 87 100                                                                    70-18 150 33 60                                                                 250 47 94                                                                      350 83 99                                                                      450 93 99                                                                     70-19 150 45 47                                                                 250 80 73                                                                      350 96 94                                                                      450 99 98                                                                   ______________________________________                                    

Remarkably high levels of herbicidal effectiveness were obtained in this test with compositions containing oleth-20 at a weight/weight ratio to glyphosate a.e. of about 1:14, and stabilized with colloidal particulates. In some cases the colloidal particulate alone contributed a major part of the efficacy enhancement. Results with composition 70-09 are out of line with other data and an application problem is suspected.

Example 71

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 71a. Concentrate compositions 71-01 to 71-04, 71-06, 71-08, 71-09, 71-11, 71-12, 71-14 and 71-16 are oil-in-water emulsion and were prepared by process (vii). Concentrate compositions 71-05, 71-07, 71-10, 71-13, 71-15 and 71-17 are aqueous solution concentrates and were prepared by process (viii).

                  TABLE 71a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl           Type of                                       composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         71-01    163       0.25     2.5    Neodol 1-12                                   71-02 163 0.25 2.5 laureth-23                                                  71-03 163 0.25 2.5 steareth-10                                                 71-04 163 0.25 2.5 steareth-20                                                 71-05 163  2.5 steareth-20                                                     71-06 163 0.25 2.5 steareth-100                                                71-07 163  2.5 steareth-100                                                    71-08 163 0.25 2.5 oleth-10                                                    71-09 163 0.25 2.5 oleth-20                                                    71-10 163  2.5 oleth-20                                                        71-11 163 0.25 2.5 ceteth-10                                                   71-12 163 0.25 2.5 ceteth-20                                                   71-13 163  2.5 ceteth-20                                                       71-14 326 0.50 5.0 ceteareth-27                                                71-15 326  5.0 ceteareth-27                                                    71-16 163 0.25 2.5 ceteareth-55                                                71-17 163  2.5 ceteareth-55                                                  ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 71b.

                  TABLE 71b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150          0        33                                            250 20 43                                                                      350 63 63                                                                      450 75 70                                                                     Formulation C 150 53 55                                                         250 80 87                                                                      350 94 97                                                                      450 98 99                                                                     Formulation J 150 40 57                                                         250 80 90                                                                      350 96 99                                                                      450 98 99                                                                     71-01 150 52 40                                                                 250 65 73                                                                      350 77 70                                                                      450 77 70                                                                     71-02 150 37 70                                                                 250 75 80                                                                      350 83 97                                                                      450 95 99                                                                     71-03 150 47 53                                                                 250 77 86                                                                      350 83 97                                                                      450 93 100                                                                    71-04 150 80 60                                                                 250 93 83                                                                      350 96 85                                                                      450 99 99                                                                     71-05 150 80 43                                                                 250 93 79                                                                      350 96 94                                                                      450 98 96                                                                     71-06 150 77 53                                                                 250 85 83                                                                      350 94 99                                                                      450 97 99                                                                     71-07 150 63 50                                                                 250 80 88                                                                      350 85 96                                                                      450 96 99                                                                     71-08 150 27 45                                                                 250 75 83                                                                      350 77 99                                                                      450 96 98                                                                     71-09 150 75 57                                                                 250 80 82                                                                      350 97 95                                                                      450 99 98                                                                     71-10 150 70 40                                                                 250 85 83                                                                      350 97 98                                                                      450 99 99                                                                     71-11 150 53 37                                                                 250 75 63                                                                      350 88 93                                                                      450 92 98                                                                     71-12 150 70 40                                                                 250 78 75                                                                      350 90 91                                                                      450 98 98                                                                     71-13 150 72 40                                                                 250 92 80                                                                      350 97 90                                                                      450 99 97                                                                     71-14 150 78 53                                                                 250 89 88                                                                      350 97 95                                                                      450 99 100                                                                    71-15 150 80 60                                                                 250 95 97                                                                      350 98 100                                                                     450 99 99                                                                     71-16 150 60 63                                                                 250 87 78                                                                      350 96 94                                                                      450 98 99                                                                     71-17 150 73 60                                                                 250 85 57                                                                      350 93 80                                                                      450 99 85                                                                   ______________________________________                                    

In combination with butyl stearate, steareth-20 (composition 71-04) gave greater herbicidal effectiveness than steareth-10 (71-03) on ABUTH. Similarly, oleth-20 (71-09) was more efficacious than oleth-10 (71-08) and ceteth-20 (71-12) than ceteth-10 (71-1). In the absence of butyl stearate, ceteareth-55 (71-17) was noticeably weaker on ECHCF than ceteareth-27 (71-15) but inclusion of butyl stearate (71-16) tended to correct this weakness. Note that while compositions 71-14 and 71-15 contained twice as high a concentration of excipients as the other compositions of the test, the concentration of glyphosate was also twice as high, thus the concentrations as sprayed were the same.

Example 72

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 72a. Concentrate compositions 72-01 to 72-05, 72-07, 72-08, 72-10 and 72-12 to 72-16 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 72-06, 72-09 and 72-11 are aqueous solution concentrates and were prepared by process (viii).

                  TABLE 72a                                                        ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate                                                                               Butyl           Type of                                       composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         72-01    163       0.25     2.5    Neodol 1-12                                   72-02 163 0.25 2.5 laureth-23                                                  72-03 163 0.25 2.5 steareth-10                                                 72-04 163 0.25 2.5 steareth-20                                                 72-05 163 0.25 2.5 Pluronic F-68                                               72-06 163  2.5 Pluronic F-68                                                   72-07 326 1.00 5.0 Pluronic F-108                                              72-08 326 0.50 5.0 Pluronic F-108                                              72-09 326  5.0 Pluronic F-108                                                  72-10 163 0.25 2.5 Pluronic F-127                                              72-11 163  2.5 Pluronic F-127                                                  72-12 326 0.50 5.0 ceteareth-27                                                72-13 163 0.25 2.5 ceteareth-55                                                72-14 163 0.25 2.5 oleth-20                                                    72-15 163 0.25 2.5 ceteth-20                                                   72-16 163 0.25 2.5 steareth-100                                              ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 72b.

                  TABLE 72b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         5          0                                            250 47  5                                                                      350 70 23                                                                      450 75 43                                                                     Formulation C 150 73 47                                                         250 99 50                                                                      350 98 67                                                                      450 99 75                                                                     Formulation J 150 73 43                                                         250 89 50                                                                      350 97 83                                                                      450 98 77                                                                     72-01 150 37 30                                                                 250 70 33                                                                      350 77 40                                                                      450 90 47                                                                     72-02 150 52 37                                                                 250 77 67                                                                      350 90 77                                                                      450 92 75                                                                     72-03 150 40 30                                                                 250 77 70                                                                      350 80 82                                                                      450 90 83                                                                     72-04 150 75 37                                                                 250 95 53                                                                      350 99 91                                                                      450 99 82                                                                     72-05 150 58 37                                                                 250 65 53                                                                      350 80 80                                                                      450 75 68                                                                     72-06 150 40 30                                                                 250 75 33                                                                      350 78 43                                                                      450 80 43                                                                     72-07 150 50 30                                                                 250 75 33                                                                      350 78 53                                                                      450 86 53                                                                     72-08 150 47 30                                                                 250 75 33                                                                      350 77 40                                                                      450 80 50                                                                     72-09 150 43 33                                                                 250 77 40                                                                      350 78 63                                                                      450 83 50                                                                     72-10 150 27 40                                                                 250 77 43                                                                      350 80 50                                                                      450 92 40                                                                     72-11 150 37 30                                                                 250 72 33                                                                      350 80 60                                                                      450 95 40                                                                     72-12 150 78 37                                                                 250 98 40                                                                      350 99 53                                                                      450 100 50                                                                    72-13 150 75 30                                                                 250 88 40                                                                      350 98 47                                                                      450 100 65                                                                    72-14 150 73 30                                                                 250 87 40                                                                      350 98 50                                                                      450 99 53                                                                     72-15 150 72 30                                                                 250 93 40                                                                      350 96 43                                                                      450 99 50                                                                     72-16 150 73 40                                                                 250 83 40                                                                      350 98 40                                                                      450 100 47                                                                  ______________________________________                                    

Composition 72-04 containing steareth-20 outperformed its counterpart 72-03 containing steareth-10, though both gave greater herbicidal effectiveness, especially on ECHCF, than 72-02 containing laureth-23 or 72-01 containing Neodol 1-12.

Example 73

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 73a. Concentrate compositions 73-01 to 73-07 and 73-09 to 73-15 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 73-08 and 73-16 are aqueous solution concentrates and were prepared by process (viii).

                  TABLE 73a                                                        ______________________________________                                         Gly-                                                                           Concentrate                                                                            phosate % w/w       Type of  Type of                                   composition                                                                            g a.e./l                                                                               Oil    Surfactant                                                                            oil      surfactant                              ______________________________________                                         73-01   163     0.5    5.0    methyl stearate                                                                         oleth-20                                  73-02 163 0.5 5.0 butyl stearate oleth-20                                      73-03 163 0.5 5.0 methyl oleate oleth-20                                       73-04 163 0.5 5.0 butyl oleate oleth-20                                        73-05 163 0.5 5.0 methyl laurate oleth-20                                      73-06 163 0.5 5.0 butyl laurate oleth-20                                       73-07 163 0.5 5.0 Orchex 796 oleth-20                                          73-08 163  5.0 none oleth-20                                                   73-09 163 0.5 5.0 methyl stearate Neodol 1-9                                   73-10 163 0.5 5.0 butyl stearate Neodol 1-9                                    73-11 163 0.5 5.0 methyl oleate Neodol 1-9                                     73-12 163 0.5 5.0 butyl oleate Neodol 1-9                                      73-13 163 0.5 5.0 methyl laurate Neodol 1-9                                    73-14 163 0.5 5.0 butyl laurate Neodol 1-9                                     73-15 163 0.5 5.0 Orchex 796 Neodol 1-9                                        73-16 163  5.0 none Neodol 1-9                                               ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 73b.

                  TABLE 73b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         3         10                                            250 58 57                                                                      350 78 53                                                                      450 77 53                                                                     Formulation C 150 60 98                                                         250 87 99                                                                      350 95 98                                                                      450 99 100                                                                    Formulation J 150 60 75                                                         250 89 87                                                                      350 93 90                                                                      450 98 99                                                                     73-01 150 75 96                                                                 250 99 97                                                                      350 97 99                                                                      450 99 100                                                                    73-02 150 60 60                                                                 250 97 67                                                                      350 99 98                                                                      450 100 95                                                                    73-03 150 63 40                                                                 250 83 82                                                                      350 97 86                                                                      450 97 88                                                                     73-04 150 73 40                                                                 250 94 82                                                                      350 97 100                                                                     450 99 100                                                                    73-05 150 67 47                                                                 250 86 67                                                                      350 97 88                                                                      450 99 100                                                                    73-06 150 60 43                                                                 250 78 91                                                                      350 97 83                                                                      450 94 86                                                                     73-07 150 70 53                                                                 250 80 53                                                                      350 97 82                                                                      450 97 92                                                                     73-08 150 70 62                                                                 250 83 83                                                                      350 91 87                                                                      450 98 98                                                                     73-09 150 45 42                                                                 250 72 72                                                                      350 77 73                                                                      450 78 89                                                                     73-10 150 40 30                                                                 250 82 80                                                                      350 78 98                                                                      450 89 93                                                                     73-11 150 40 30                                                                 250 65 60                                                                      350 77 90                                                                      450 96 92                                                                     73-12 150 20 30                                                                 250 63 73                                                                      350 80 75                                                                      450 93 86                                                                     73-13 150 20 27                                                                 250 67 60                                                                      350 82 91                                                                      450 88 92                                                                     73-14 150 7 30                                                                  250 72 81                                                                      350 87 78                                                                      450 80 85                                                                     73-15 150 20 23                                                                 250 65 60                                                                      350 77 81                                                                      450 87 88                                                                     73-16 150 12 30                                                                 250 57 53                                                                      350 68 85                                                                      450 85 85                                                                   ______________________________________                                    

Composition 73-08, containing as sole excipient substance oleth-20 at a 1:3 weight/weight ratio to glyphosate a.e., exhibited high herbicidal effectiveness, at least equal to commercial standard Formulations C and J on ABUTH but a little weaker on ECHCF. By comparison, composition 73-16, wherein the sole excipient substance was Neodol 1-9 at the same ratio to glyphosate, had much weaker activity. Addition of a small amount of fatty acid ester in most cases enhanced effectiveness, especially on ECHCF. In this study the most efficacious composition was 73-01, containing oleth-20 and methyl stearate. When added to Neodol 1-9, butyl stearate was more efficacious than methyl stearate, methyl oleate or butyl oleate. The mineral oil Orchex 796 did not substitute effectively for butyl stearate, either with oleth-20 or with Neodol 1-9.

Example 74

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 74a. Concentrate compositions 74-01, 74-03, 74-05 to 74-08, 74-10 and 74-14 to 74-17 are oil-in-water emulsions prepared by process (vii). Concentrate compositions 74-02, 74-04, 74-09 and 74-11 to 74-13 are aqueous solution concentrates and were prepared by process (viii). Some compositions contained a coupling agent as indicated in Table 74a; the coupling agent was added with the surfactant.

                                      TABLE 74a                                    __________________________________________________________________________               % w/w                                                                Conc.                                                                              Glyphosate                                                                           Butyl    Coupling                                                                            Type of Type of                                          comp. g a.e./l stearate Surfactant agent coupling agent surfactant           __________________________________________________________________________     74-01                                                                              326   1.0 5.0  2.5  Arcosolve DPM                                                                          oleth-20                                         74-02 326  5.0 2.5 Arcosolve DPM oleth-20                                      74-03 163 0.5 2.5  none oleth-20                                               74-04 163  2.5  none oleth-20                                                  74-05 326 1.0 5.0  none ceteareth-27                                           74-06 326 1.0 5.0 2.5 PEG-400 ceteareth-27                                     74-07 326 1.0 5.0 2.5 Dowanol TPNB ceteareth-27                                74-08 326 1.0 5.0 2.5 Dowanol PNB ceteareth-27                                 74-09 163  2.5  none ceteareth-27                                              74-10 326 0.5 5.0  none ceteareth-27                                           74-11 326  5.0 2.5 PEG-400 ceteareth-27                                        74-12 326  5.0 2.5 Dowanol TPNB ceteareth-27                                   74-13 326  5.0 2.5 Dowanol PNB ceteareth-27                                    74-14 163 0.5 2.5  none Neodol 1-9                                             74-15 163 0.5 2.5  none laureth-23                                             74-16 163 0.5 2.5  none steareth-20                                            74-17 163 0.5 2.5  none ceteareth-27                                         __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 74b.

                  TABLE 74b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         0         5                                             250 38 20                                                                      350 63 30                                                                      450 70 70                                                                     Formulation C 150 70 75                                                         250 92 94                                                                      350 99 99                                                                      450 99 98                                                                     Formulation J 150 65 50                                                         250 88 92                                                                      350 97 99                                                                      450 98 97                                                                     74-01 150 58 83                                                                 250 77 88                                                                      350 93 96                                                                      450 93 99                                                                     74-02 150 40 76                                                                 250 75 100                                                                     350 92 100                                                                     450 92 100                                                                    74-03 150 48 75                                                                 250 83 96                                                                      350 92 100                                                                     450 99 100                                                                    74-04 150 40 82                                                                 250 78 99                                                                      350 87 99                                                                      450 98 100                                                                    74-05 150 68 92                                                                 250 87 99                                                                      350 95 99                                                                      450 99 99                                                                     74-06 150 55 60                                                                 250 83 99                                                                      350 97 99                                                                      450 98 98                                                                     74-07 150 63 57                                                                 250 80 96                                                                      350 95 97                                                                      450 99 98                                                                     74-08 150 73 75                                                                 250 90 90                                                                      350 95 97                                                                      450 100 97                                                                    74-09 150 73 68                                                                 250 87 73                                                                      350 92 90                                                                      450 97 95                                                                     74-10 150 70 63                                                                 250 87 80                                                                      350 98 94                                                                      450 99 96                                                                     74-11 150 73 60                                                                 250 90 77                                                                      350 99 93                                                                      450 100 95                                                                    74-12 150 72 67                                                                 250 83 75                                                                      350 90 82                                                                      450 99 94                                                                     74-13 150 73 70                                                                 250 80 83                                                                      350 99 94                                                                      450 100 92                                                                    74-14 150 5 20                                                                  250 55 63                                                                      350 77 93                                                                      450 78 99                                                                     74-15 150 43 57                                                                 250 78 88                                                                      350 88 98                                                                      450 90 98                                                                     74-16 150 65 57                                                                 250 83 82                                                                      350 88 98                                                                      450 95 97                                                                     74-17 150 72 50                                                                 250 80 93                                                                      350 88 90                                                                      450 95 97                                                                   ______________________________________                                    

The superiority of herbicidal effectiveness provided by C₁₆₋₁₈ alkylethers (oleth-20, ceteareth-27, steareth-20) over that provided by shorter chain alkylethers (Neodol 1-9, laureth-23) was very pronounced in this test.

Example 75

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 75a. Concentrate compositions 75-01 to 75-07 and 75-09 to 75-15 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 75-08 and 75-16 are aqueous solution concentrates and were prepared by process (viii).

                  TABLE 75a                                                        ______________________________________                                         Gly-                                                                           Concentrate                                                                            phosate % w/w       Type of  Type of                                   composition                                                                            g a.e./l                                                                               Oil    Surfactant                                                                            oil      surfactant                              ______________________________________                                         75-01   163     0.5    5.0    methyl stearate                                                                         steareth-20                               75-02 163 0.5 5.0 butyl stearate steareth-20                                   75-03 163 0.5 5.0 methyl oleate steareth-20                                    75-04 163 0.5 5.0 butyl oleate steareth-20                                     75-05 163 0.5 5.0 methyl laurate steareth-20                                   75-06 163 0.5 5.0 butyl laurate steareth-20                                    75-07 163 0.5 5.0 Orchex 796 steareth-20                                       75-08 163  5.0 none steareth-20                                                75-09 163 0.5 5.0 methyl stearate ceteareth-27                                 75-10 163 0.5 5.0 butyl stearate ceteareth-27                                  75-11 163 0.5 5.0 methyl oleate ceteareth-27                                   75-12 163 0.5 5.0 butyl oleate ceteareth-27                                    75-13 163 0.5 5.0 methyl laurate ceteareth-27                                  75-14 163 0.5 5.0 butyl laurate ceteareth-27                                   75-15 163 0.5 5.0 Orchex 796 ceteareth-27                                      75-16 163  5.0 none ceteareth-27                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 75b.

                  TABLE 75b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         15         5                                            250 57 20                                                                      350 83 50                                                                      450 78 73                                                                     Formulation C 150 65 63                                                         250 87 93                                                                      350 92 94                                                                      450 98 100                                                                    Formulation J 150 50 73                                                         250 90 90                                                                      350 94 98                                                                      450 98 99                                                                     75-01 150 72 70                                                                 250 88 85                                                                      350 96 83                                                                      450 99 86                                                                     75-02 150 73 53                                                                 250 83 87                                                                      350 97 99                                                                      450 97 98                                                                     75-03 150 68 33                                                                 250 87 92                                                                      350 93 97                                                                      450 98 93                                                                     75-04 150 72 50                                                                 250 87 88                                                                      350 94 86                                                                      450 98 97                                                                     75-05 150 72 67                                                                 250 83 82                                                                      350 99 97                                                                      450 98 98                                                                     75-06 150 73 33                                                                 250 95 83                                                                      350 99 95                                                                      450 99 88                                                                     75-07 150 73 55                                                                 250 93 73                                                                      350 95 83                                                                      450 98 91                                                                     75-08 150 75 40                                                                 250 94 60                                                                      350 98 86                                                                      450 99 92                                                                     75-09 150 77 50                                                                 250 90 50                                                                      350 98 92                                                                      450 99 98                                                                     75-10 150 72 53                                                                 250 92 77                                                                      350 96 86                                                                      450 99 99                                                                     75-11 150 72 60                                                                 250 87 87                                                                      350 97 97                                                                      450 97 99                                                                     75-12 150 70 57                                                                 250 90 90                                                                      350 96 96                                                                      450 98 99                                                                     75-13 150 68 40                                                                 250 90 77                                                                      350 99 95                                                                      450 99 98                                                                     75-14 150 77 33                                                                 250 94 70                                                                      350 96 82                                                                      450 99 93                                                                     75-15 150 75 30                                                                 250 96 75                                                                      350 97 88                                                                      450 99 92                                                                     75-16 150 77 40                                                                 250 99 47                                                                      350 98 67                                                                      450 98 78                                                                   ______________________________________                                    

Steareth-20 and ceteareth-27, as sole excipient substances (compositions 75-08 and 75-16 respectively) provided excellent herbicidal effectiveness, but further enhancements, especially on ECHCF, were obtained by inclusion of a small amount of fatty acid ester in the composition.

Example 76

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 76a. Concentrate compositions 76-13 and 76-14 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 76-01 to 76-12 and 76-15 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix). Concentrate compositions 76-16 and 76-17 contained colloidal particulates but no surfactant.

Compositions 76-13 and 76-14 (both containing 162 g a.e./l glyphosate) showed acceptable storage stability. However, at glyphosate loadings>480 g a.e./l (as in compositions 76-01 to 76-12 and 76-15) storage-stable compositions containing 3% oleth-20 could not be made except with the addition of colloidal particulate as shown below.

                  TABLE 76a                                                        ______________________________________                                         Gly-        % w/w                                                              Concentrate                                                                            phosate Oleth-               Type of                                     composition g a.e./l 20 Glycerin Aerosil Aerosil                             ______________________________________                                         76-01   492     3.00    2.0    0.8   380                                         76-02 492 3.00 5.0 1.5 380                                                     76-03 492 3.00 2.0 0.8 380                                                     76-04 492 3.00 5.0 1.5 380                                                     76-05 492 3.00  0.8 OX-50                                                      76-06 492 3.00  1.5 OX-50                                                      76-07 492 3.00  0.8 380/OX-50 blend                                            76-08 492 3.00  1.5 380/OX-50 blend                                            76-09 492 3.00  0.8 380                                                        76-10 492 3.00  1.5 380                                                        76-11 492 3.00  0.8 380                                                        76-12 492 3.00  1.5 380                                                        76-13 162 1.13   none                                                          76-14 162 1.13   none                                                          76-15 492 3.00 2.0 1.5 380                                                     76-16 488   0.8 380                                                            76-17 488   1.5 380                                                          ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 76b.

                  TABLE 76b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         18        40                                            250 57 53                                                                      350 72 63                                                                      450 83 85                                                                     Formulation J 150 70 65                                                         250 85 95                                                                      350 98 98                                                                      450 100 99                                                                    76-01 150 62 67                                                                 250 72 93                                                                      350 99 96                                                                      450 99 97                                                                     76-02 150 57 50                                                                 250 70 91                                                                      350 92 97                                                                      450 99 99                                                                     76-03 150 48 40                                                                 250 68 67                                                                      350 97 97                                                                      450 98 98                                                                     76-04 150 55 50                                                                 250 82 83                                                                      350 95 90                                                                      450 99 94                                                                     76-05 150 65 43                                                                 250 87 87                                                                      350 100 94                                                                     450 96 95                                                                     76-06 150 55 53                                                                 250 75 82                                                                      350 95 95                                                                      450 100 96                                                                    76-07 150 45 83                                                                 250 78 82                                                                      350 90 93                                                                      450 95 99                                                                     76-08 150 55 47                                                                 250 75 88                                                                      350 93 99                                                                      450 99 97                                                                     76-09 150 47 47                                                                 250 65 82                                                                      350 78 99                                                                      450 97 97                                                                     76-10 150 47 40                                                                 250 72 96                                                                      350 77 80                                                                      450 85 97                                                                     76-11 150 37 53                                                                 250 73 82                                                                      350 80 83                                                                      450 90 92                                                                     76-12 150 35 57                                                                 250 70 82                                                                      350 80 97                                                                      450 90 99                                                                     76-13 150 50 40                                                                 250 68 75                                                                      350 95 92                                                                      450 99 95                                                                     76-14 150 40 33                                                                 250 70 82                                                                      350 93 89                                                                      450 98 93                                                                     76-15 150 23 33                                                                 250 67 73                                                                      350 83 91                                                                      450 94 92                                                                     76-16 150 13 40                                                                 250 45 50                                                                      350 62 72                                                                      450 77 77                                                                     76-17 150 7 33                                                                  250 50 50                                                                      350 60 70                                                                      450 75 73                                                                   ______________________________________                                    

Several high-loaded (492 g a.e./l) glyphosate compositions containing oleth-20 at just 3% exhibited surprisingly high herbicidal effectiveness, approaching or equaling that of commercial standard Formulation J, which is loaded at only about 360 g a.e./l and has a much higher surfactant to glyphosate ratio.

Example 77

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 77a. Concentrate composition 77-08 to 77-14 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 77-15 to 77-17 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 77-01 to 77-07 contain colloidal particulates and were prepared by process (ix).

Compositions 77-08 to 77-17 (all containing 163 g a.e./l glyphosate) showed acceptable storage stability. However, at a glyphosate loading of 400 g a.e./l (as in compositions 77-01 to 77-07) storage-stable compositions containing 0.5-1% butyl stearate and 5-10% alkylether surfactant could not be made except with the addition of colloidal particulate as shown below.

                  TABLE 77a                                                        ______________________________________                                         Gly-        % w/w                                                              Concentrate                                                                            phosate Butyl                 Type of                                    composition g a.e./l stearate Surfactant Aerosil 90 surfactant               ______________________________________                                         77-01   400     1.0     10.0   1.0    ceteareth-27                               77-02 400 1.0 10.0 1.0 steareth-20                                             77-03 400 0.5 5.0 1.0 ceteareth-27                                             77-04 400 0.5 5.0 1.0 steareth-20                                              77-05 400 1.0 5.0 1.0 ceteareth-27                                             77-06 400 1.0 5.0 1.0 steareth-20                                              77-07 400 1.0 5.0 1.0 steareth-30                                              77-08 163 0.5 5.0  oleth-20                                                    77-09 163 0.5 5.0  steareth-20                                                 77-10 163 0.5 5.0  ceteth-20                                                   77-11 163 0.5 5.0  laureth-23                                                  77-12 163 0.5 5.0  ceteareth-27                                                77-13 163 0.5 5.0  Neodol 25-12                                                77-14 163 0.5 5.0  Neodol 25-20                                                77-15 163  5.0  steareth-20                                                    77-16 163  5.0  ceteth-20                                                      77-17 163  5.0  laureth-23                                                   ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 77b.

                  TABLE 77b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate applied                                                                          g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         0         40                                            250 20 60                                                                      350 68 82                                                                      450 83 96                                                                     Formulation C 150 68 93                                                         250 93 99                                                                      350 100 100                                                                    450 100 100                                                                   Formulation J 150 43 89                                                         250 93 100                                                                     350 100 100                                                                    450 100 100                                                                   77-01 150 78 97                                                                 250 96 100                                                                     350 98 100                                                                     450 100 100                                                                   77-02 150 91 98                                                                 250 100 100                                                                    350 100 100                                                                    450 100 100                                                                   77-03 150 90 97                                                                 250 99 99                                                                      350 100 100                                                                    450 100 100                                                                   77-04 150 77 98                                                                 250 100 100                                                                    350 100 100                                                                    450 100 100                                                                   77-05 150 82 93                                                                 250 100 99                                                                     350 100 100                                                                    450 100 100                                                                   77-06 150 83 85                                                                 250 100 99                                                                     350 100 100                                                                    450 100 100                                                                   77-07 150 83 87                                                                 250 100 100                                                                    350 100 100                                                                    450 100 100                                                                   77-08 150 90 92                                                                 250 100 100                                                                    350 100 100                                                                    450 100 100                                                                   77-09 150 90 85                                                                 250 100 98                                                                     350 100 100                                                                    450 100 100                                                                   77-10 150 80 85                                                                 250 100 92                                                                     350 100 100                                                                    450 100 100                                                                   77-11 150 83 88                                                                 250 96 99                                                                      350 100 98                                                                     450 100 100                                                                   77-12 150 93 85                                                                 250 100 99                                                                     350 100 100                                                                    450 100 100                                                                   77-13 150 72 73                                                                 250 92 97                                                                      350 100 99                                                                     450 100 100                                                                   77-14 150 72 80                                                                 250 99 99                                                                      350 100 100                                                                    450 100 100                                                                   77-15 150 100 93                                                                250 100 99                                                                     350 100 100                                                                    450 100 100                                                                   77-16 150 100 98                                                                250 100 100                                                                    350 100 100                                                                    450 100 100                                                                   77-17 150 83 83                                                                 250 100 99                                                                     350 100 99                                                                     450 100 99                                                                  ______________________________________                                    

Outstanding herbicidal effectiveness was provided by compositions containing C₁₆₋₁₈ alkylether surfactants (ceteareth-27, steareth-20, steareth-30, oleth-20, ceteth-20). High-loaded (400 g a.e./l) glyphosate compositions containing a C₁₆₋₁₈ alkylether surfactant, butyl stearate and a colloidal particulate (Aerosil 90) to stabilize the compositions performed especially impressively in this test.

Example 78

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 78a. Concentrate composition 78-01 to 78-09, 78-11 to 78-14, 78-16 and 78-17 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 78-10 and 78-15 are aqueous solution concentrates and were prepared by process (viii).

                                      TABLE 78a                                    __________________________________________________________________________               % w/w                                                                Conc.                                                                              Glyphosate                                                                              Oleth-                                                                             Other                                                                               Type of  Other                                             comp. g a.e./l Oil 20 surfactant oil surfactant                              __________________________________________________________________________     78-01                                                                              163   0.25                                                                              2.5      methyl laurate                                             78-02 163 0.25 2.5  methyl myristate                                           78-03 163 0.25 2.5  methyl palmitoleate                                        78-04 163 0.25 2.5  methyl palmitate                                           78-05 163 0.25 2.5  methyl linoleate                                           78-06 163 0.25 2.5  methyl oleate                                              78-07 163 0.25 2.5  methyl stearate                                            78-08 163 0.25 2.5  ethyl stearate                                             78-09 163 0.25 2.5  butyl stearate                                             78-10 163  2.5  none                                                           78-11 163 0.25  2.5 methyl palmitoleate MON 0818                               78-12 163 0.25  2.5 methyl palmitate MON 0818                                  78-13 163 0.25  2.5 methyl oleate MON 0818                                     78-14 163 0.25  2.5 methyl stearate MON 0818                                   78-15 163   2.5 none MON 0818                                                  78-16 163 0.25  2.5 butyl stearate laureth-23                                  78-17 163 0.25  2.5 butyl stearate Neodol 1-9                                __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 20 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 78b.

                  TABLE 78b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          2        35                                            200 52 67                                                                      300 77 83                                                                      400 78 87                                                                     Formulation C 100 25 77                                                         200 72 99                                                                      300 87 100                                                                     400 99 100                                                                    Formulation J 100 13 73                                                         200 70 97                                                                      300 90 100                                                                     400 97 100                                                                    78-01 100 22 55                                                                 200 65 86                                                                      300 78 98                                                                      400 89 98                                                                     78-02 100 20 63                                                                 200 67 91                                                                      300 83 99                                                                      400 97 100                                                                    78-03 100 30 75                                                                 200 63 98                                                                      300 83 99                                                                      400 94 100                                                                    78-04 100 23 63                                                                 200 60 98                                                                      300 90 99                                                                      400 95 100                                                                    78-05 100 27 57                                                                 200 62 91                                                                      300 83 96                                                                      400 93 98                                                                     78-06 100 23 50                                                                 200 63 89                                                                      300 83 99                                                                      400 96 99                                                                     78-07 100 25 53                                                                 200 65 94                                                                      300 83 99                                                                      400 92 99                                                                     78-08 100 13 47                                                                 200 53 88                                                                      300 89 97                                                                      400 95 99                                                                     78-09 100 27 53                                                                 200 60 85                                                                      300 83 97                                                                      400 97 98                                                                     78-10 100 13 53                                                                 200 62 94                                                                      300 83 97                                                                      400 88 99                                                                     78-11 100 23 60                                                                 200 50 90                                                                      300 85 98                                                                      400 95 99                                                                     78-12 100 17 55                                                                 200 35 94                                                                      300 78 98                                                                      400 94 99                                                                     78-13 100  8 50                                                                 200 43 90                                                                      300 73 98                                                                      400 90 99                                                                     78-14 100 30 63                                                                 200 45 92                                                                      300 80 98                                                                      400 94 98                                                                     78-15 100 20 63                                                                 200 70 96                                                                      300 82 99                                                                      400 94 98                                                                     78-16 100 18 62                                                                 200 62 83                                                                      300 80 97                                                                      400 97 97                                                                     78-17 100 17 52                                                                 200 58 85                                                                      300 75 90                                                                      400 95 98                                                                   ______________________________________                                    

Not great or consistent enhancement of herbicidal effectiveness of glyphosate compositions containing oleth-20 was obtained by adding a small amount of any of a variety of fatty acid esters in this study (compare 78-10 with 78-01 to 78-09).

Example 79

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 79a. Concentrate composition 79-01 to 79-09, 79-11 to 79-14, 79-16 and 79-17 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 79-10 and 79-15 are aqueous solution concentrates and were prepared by process (viii).

                                      TABLE 79a                                    __________________________________________________________________________                 % w/w                                                              Concentrate                                                                          Glyphosate                                                                               Oleth-                                                                             Other                                                                               Type of  Other                                          composition g a.e./l Oil 20 surfactant oil surfactant                        __________________________________________________________________________     79-01 163   0.25                                                                               2.5      isopropyl myristate                                     79-02 163 0.25 2.5  ethyl myristate                                            79-03 163 0.25 2.5  methyl palmitate                                           79-04 163 0.25 2.5  ethyl palmitate                                            79-05 163 0.25 2.5  ethyl linoleate                                            79-06 163 0.25 2.5  ethyl oleate                                               79-07 163 0.25 2.5  methyl stearate                                            79-08 163 0.25 2.5  ethyl stearate                                             79-09 163 0.25 2.5  butyl stearate                                             79-10 163  2.5  none                                                           79-11 163 0.25  2.5 methyl palmitate MON 0818                                  79-12 163 0.25  2.5 methyl stearate MON 0818                                   79-13 163 0.25  2.5 ethyl stearate MON 0818                                    79-14 163 0.25  2.5 ethyl oleate MON 0818                                      79-15 163   2.5 none MON 0818                                                  79-16 163 0.25  2.5 butyl stearate laureth-23                                  79-17 163 0.25  2.5 butyl stearate Neodol 1-9                                __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 79b.

                  TABLE 79b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         12        33                                            200 45 43                                                                      300 73 63                                                                      400 80 63                                                                     Formulation C 100 43 57                                                         200 75 88                                                                      300 95 99                                                                      400 100 99                                                                    Formulation J 100 53 60                                                         200 77 75                                                                      300 96 95                                                                      400 99 98                                                                     79-01 100 35 40                                                                 200 73 72                                                                      300 83 91                                                                      400 99 97                                                                     79-02 100 38 30                                                                 200 70 43                                                                      300 87 82                                                                      400 96 80                                                                     79-03 100 25 27                                                                 200 68 50                                                                      300 90 73                                                                      400 96 82                                                                     79-04 100 27 27                                                                 200 75 50                                                                      300 80 73                                                                      400 96 80                                                                     79-05 100 33 27                                                                 200 68 43                                                                      300 83 70                                                                      400 97 91                                                                     79-06 100 33 28                                                                 200 72 53                                                                      300 83 60                                                                      400 99 70                                                                     79-07 100 37 25                                                                 200 72 40                                                                      300 83 50                                                                      400 97 65                                                                     79-08 100 32 25                                                                 200 73 43                                                                      300 87 60                                                                      400 98 67                                                                     79-09 100 35 25                                                                 200 75 43                                                                      300 95 57                                                                      400 98 63                                                                     79-10 100 35 27                                                                 200 73 40                                                                      300 83 76                                                                      400 97 73                                                                     79-11 100 35 33                                                                 200 67 67                                                                      300 80 86                                                                      400 92 70                                                                     79-12 100 25 30                                                                 200 67 70                                                                      300 83 76                                                                      400 88 80                                                                     79-13 100 27 33                                                                 200 70 66                                                                      300 78 63                                                                      400 93 60                                                                     79-14 100 33 30                                                                 200 67 47                                                                      300 80 70                                                                      400 92 77                                                                     79-15 100 20 30                                                                 200 68 40                                                                      300 83 75                                                                      400 90 72                                                                     79-16 100 30 25                                                                 200 62 43                                                                      300 73 73                                                                      400 77 70                                                                     79-17 100 30 23                                                                 200 58 40                                                                      300 75 60                                                                      400 80 73                                                                   ______________________________________                                    

In this study, isopropyl myristate (composition 79-01) was the most effective of the fatty acid esters tested as additives to oleth-20 (79-10) in glyphosate compositions.

Example 80

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 80a. Concentrate composition 80-01 to 80-13 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 80-14 to 80-17 are aqueous solution concentrates and were prepared by process (viii).

                  TABLE 80a                                                        ______________________________________                                         Gly-        % w/w                                                              Concentrate                                                                            phosate        Surf-                                                                               Type of   Type of                                    composition g a.e./l Oil actant oil surfactant                               ______________________________________                                         80-01   163     0.25   2.5  butyl stearate                                                                           laureth-23                                 80-02 163 0.25 2.5 butyl stearate steareth-20                                  80-03 163 0.25 2.5 butyl stearate ceteareth-20                                 80-04 163 0.25 2.5 butyl stearate ceteareth-15                                 80-05 163 0.25 2.5 butyl stearate Neodol 45-13                                 80-06 163 0.25 2.5 methyl stearate steareth-20                                 80-07 163 0.25 2.5 methyl stearate ceteareth-20                                80-08 163 0.25 2.5 methyl stearate ceteareth-15                                80-09 163 0.25 2.5 methyl stearate Neodol 45-13                                80-10 163 0.25 2.5 methyl palmitate steareth-20                                80-11 163 0.25 2.5 methyl palmitate ceteareth-20                               80-12 163 0.25 2.5 methyl palmitate ceteareth-15                               80-13 163 0.25 2.5 methyl palmitate Neodol 45-13                               80-14 163  2.5 none steareth-20                                                80-15 163  2.5 none ceteareth-20                                               80-16 163  2.5 none ceteareth-15                                               80-17 163  2.5 none Neodol 45-13                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 24 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 80b.

                  TABLE 80b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         10        37                                            200 30 40                                                                      300 43 57                                                                      400 23 33                                                                     Formulation C 100 50 67                                                         200 75 96                                                                      300 85 99                                                                      400 94 100                                                                    Formulation J 100 40 75                                                         200 73 94                                                                      300 93 98                                                                      400 95 99                                                                     80-01 100 63 77                                                                 200 67 94                                                                      300 77 99                                                                      400 88 96                                                                     80-02 100 63 75                                                                 200 83 88                                                                      300 93 98                                                                      400 95 99                                                                     80-03 100 67 75                                                                 200 82 95                                                                      300 95 99                                                                      400 98 99                                                                     80-04 100 60 75                                                                 200 82 97                                                                      300 96 99                                                                      400 98 100                                                                    80-05 100 63 73                                                                 200 75 89                                                                      300 80 98                                                                      400 87 97                                                                     80-06 100 58 63                                                                 200 78 93                                                                      300 93 99                                                                      400 98 100                                                                    80-07 100 60 67                                                                 200 78 93                                                                      300 93 99                                                                      400 100  99                                                                   80-08 100 missing missing                                                       200 missing missing                                                            300 78 95                                                                      400 98 99                                                                     80-09 100 23 30                                                                 200 65 83                                                                      300 80 98                                                                      400 93 99                                                                     80-10 100 65 67                                                                 200 83 95                                                                      300 97 99                                                                      400 99 99                                                                     80-11 100 72 73                                                                 200 90 98                                                                      300 96 97                                                                      400 99 99                                                                     80-12 100 68 63                                                                 200 90 92                                                                      300 98 99                                                                      400 97 99                                                                     80-13 100 43 73                                                                 200 72 87                                                                      300 83 98                                                                      400 93 96                                                                     80-14 100 62 77                                                                 200 78 99                                                                      300 95 99                                                                      400 98 100                                                                    80-15 100 52 60                                                                 200 78 93                                                                      300 94 98                                                                      400 97 99                                                                     80-16 100 38 68                                                                 200 68 99                                                                      300 87 97                                                                      400 94 99                                                                     80-17 100 55 75                                                                 200 68 91                                                                      300 83 96                                                                      400 87 98                                                                   ______________________________________                                    

Herbicidal effectiveness exceeding that of commercial standard composition J, at least on ABUTH, was recorded with several compositions, including 80-02 (steareth-20 plus butyl stearate), 80-03 (ceteareth-20 plus butyl stearate), 80-04 (ceteareth-15 plus butyl stearate), 80-10 (steareth-20 plus methyl palmitate), 80-11 (ceteareth-20 plus methyl palmitate) and 80-12 (ceteareth-15 plus methyl palmitate). Compositions lacking fatty acid ester performed slightly less well overall than those containing butyl stearate or methyl palmitate.

Example 81

Spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 81a. Compositions were prepared by simple mixing of ingredients. Soybean lecithin (45% phospholipid, Avanti), where included, was first prepared with sonication in water to make a homogeneous composition. Four different concentrations of glyphosate (not shown in Table 81a) were prepared, calculated to provide, when applied in a spray volume of 93 l/ha, the glyphosate rates shown in Table 81b.

                                      TABLE 81a                                    __________________________________________________________________________     % w/w                                                                          Spray       Butyl                                                                              Methyl                                                                             Oleth-                                                                             Lecithin                                                                               Methyl oleate                                    comp. Lecithin FC-754 stearate oleate 20 supplied as supplied as             __________________________________________________________________________     81-01                                                                              0.05                                                                               0.050           soybean lecithin                                         81-02 0.05  0.050   soybean lecithin                                           81-03 0.05     soybean lecithin                                                81-04  0.050                                                                   81-05   0.050                                                                  81-06 0.05     LI-700                                                          81-07   0.005  0.05                                                            81-08    0.01 0.05                                                             81-09     0.05                                                                 81-10   0.005                                                                  81-11    0.01   pure                                                           81-12    0.01   methylated seed oil                                          __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and Prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 14 days after planting ECHCF and 21 days after planting SIDSP. Evaluation of herbicidal inhibition was done 14 days after application.

Formulations B and C were applied as comparative treatments, representing technical glyphosate IPA salt and a commercial formulation of glyphosate IPA salt respectively. Results, averaged for all replicates of each treatment, are shown in Table 81b.

                  TABLE 81b                                                        ______________________________________                                                     Glyphosate rate                                                                           % Inhibition                                            Composition applied                                                                        g a.e./ha  ABUTH    ECHCF  SIDSP                                   ______________________________________                                         Formulation B                                                                              50         0        0      0                                         (technical) 100 38 35 35                                                        200 87 50 90                                                                   300 95 88 94                                                                  Formulation C 50 0 2 0                                                         (commercial) 100 32 55 25                                                       200 85 97 93                                                                   300 96 99 96                                                                  81-01 50 78 53 88                                                               100 90 60 95                                                                   200 99 96 99                                                                   300 99 97 98                                                                  81-02 50 25 15 43                                                               100 72 30 82                                                                   200 94 62 93                                                                   300 95 77 94                                                                  81-03 50 20 8 32                                                                100 52 22 78                                                                   200 87 55 91                                                                   300 95 65 93                                                                  81-04 50 62 37 85                                                               100 82 68 92                                                                   200 97 96 95                                                                   300 98 95 97                                                                  81-05 50 15 10 25                                                               100 47 27 23                                                                   200 85 62 87                                                                   300 90 63 92                                                                  81-06 50 0 2 0                                                                  100 20 15 20                                                                   200 85 60 82                                                                   300 90 65 90                                                                  81-07 50 67 27 82                                                               100 87 55 93                                                                   200 94 92 96                                                                   300 97 99 97                                                                  81-08 50 62 30 75                                                               100 78 63 91                                                                   200 93 96 96                                                                   300 94 98 98                                                                  81-09 50 65 45 77                                                               100 80 73 95                                                                   200 93 98 97                                                                   300 95 99 99                                                                  81-10 50 10 25 5                                                                100 23 35 37                                                                   200 90 50 93                                                                   300 92 73 94                                                                  81-11 50 10 25 0                                                                100 52 33 43                                                                   200 88 72 93                                                                   300 94 78 94                                                                  81-12 50 0 15 0                                                                 100 43 35 33                                                                   200 91 70 90                                                                   300 94 82 93                                                                ______________________________________                                    

Results of this test using glyphosate as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (81-03) was a much more effective excipient than the lecithin-based adjuvant LI-700 (81-06) widely used in the art.

Butyl stearate alone at 0.05% (81-05) did not greatly enhance effectiveness.

The combination of lecithin and butyl stearate (81-02) gave surprisingly strong enhancement of effectiveness, suggesting a synergistic interaction between these two excipient substances.

Fluorad FC-754, either alone (81-04) or in combination with lecithin (81-01) gave extremely high effectiveness, superior to that obtained with the commercial standard.

Oleth-20 at the low concentration of 0.05% (81-09) gave extremely high effectiveness, superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (81-07) or 0.01% methyl oleate (81-08) did not provide further enhancement.

Example 82

Spray compositions were prepared containing paraquat dichloride and excipient ingredients. Compositions 82-01 to 82-12 were exactly like compositions 81-01 to 81-12 except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 8 days after planting ECHCF and 21 days after planting SIDSP. Evaluation of herbicidal inhibition was done 12 days after application.

Standards included technical paraquat dichloride and Gramoxone, a commercial formulation of paraquat from Zeneca. Results, averaged for all replicates of each treatment, are shown in Table 82.

                  TABLE 82                                                         ______________________________________                                                     Paraquat rate                                                                            % Inhibition                                             Spray composition                                                                          g a.i./ha ABUTH    ECHCF  SIDSP                                    ______________________________________                                         Paraquat dichloride                                                                        25        50       83     55                                         (technical) 50 57 78 60                                                         100 73 84 69                                                                   200 85 95 99                                                                  Gramoxone 25 40 72 40                                                          (commercial) 50 60 70 52                                                        100 72 58 55                                                                   200 72 89 63                                                                  82-01 25 75 93 67                                                               50 82 97 91                                                                    100 95 98 97                                                                   200 100 99 99                                                                 82-02 25 67 80 48                                                               50 68 87 65                                                                    100 88 97 93                                                                   200 96 99 98                                                                  82-03 25 55 65 42                                                               50 62 87 65                                                                    100 83 96 93                                                                   200 95 99 97                                                                  82-04 25 53 82 45                                                               50 63 94 53                                                                    100 88 99 86                                                                   200 92 99 98                                                                  82-05 25 58 67 50                                                               50 60 62 45                                                                    100 70 73 62                                                                   200 85 90 88                                                                  82-06 25 53 77 43                                                               50 60 92 40                                                                    100 80 93 55                                                                   200 96 99 78                                                                  82-07 25 65 80 45                                                               50 82 92 70                                                                    100 96 96 89                                                                   200 100 98 99                                                                 82-08 25 67 80 37                                                               50 82 90 71                                                                    100 97 98 65                                                                   200 99 99 93                                                                  82-09 25 72 90 50                                                               50 80 97 57                                                                    100 91 99 94                                                                   200 97 100 97                                                                 82-10 25 67 87 45                                                               50 68 75 57                                                                    100 78 93 63                                                                   200 82 97 82                                                                  82-11 25 65 80 45                                                               50 73 77 62                                                                    100 90 95 62                                                                   200 94 98 78                                                                  82-12 25 67 78 37                                                               50 75 90 55                                                                    100 77 97 90                                                                   200 85 99 92                                                                ______________________________________                                    

Results of this test using paraquat as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (82-03) was a much more effective excipient on SIDSP than the lecithin-based adjuvant LI-700 (82-06) widely used in the art.

Butyl stearate alone at 0.05% (82-05) did not enhance effectiveness.

The combination of lecithin and butyl stearate (82-02) gave surprisingly strong enhancement of effectiveness, suggesting a synergistic interaction between these two excipient substances.

Fluorad FC-754 (82-04) gave extremely high effectiveness, superior to that obtained with the commercial standard. In the presence of lecithin (82-01), effectiveness was further increased dramatically, suggesting a synergistic interaction between these two excipient substances.

Oleth-20 at the low concentration of 0.05% (82-09) gave extremely high effectiveness, superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (82-07) or 0.01% methyl oleate (82-08) did not provide further enhancement.

Example 83

Spray compositions were prepared containing acifluorfen sodium salt and excipient ingredients. Compositions 83-01 to 83-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 15 days after planting ABUTH, 9 days after planting ECHCF and 22 days after planting SIDSP. Evaluation of herbicidal inhibition was done 10 days after application.

Standards included technical acifluorfen sodium and Blazer, a commercial formulation of acifluorfen from Rohm & Haas. Results, averaged for all replicates of each treatment, are shown in Table 83.

                  TABLE 83                                                         ______________________________________                                                    Acifluorfen rate                                                                           % Inhibition                                            Spray composition                                                                         g a.i./ha   ABUTH    ECHCF  SIDSP                                   ______________________________________                                         Acifluorfen                                                                               25          20       2      15                                        (technical) 50 32 7 17                                                          100 52 18 35                                                                   200 62 35 40                                                                  Blazer 25 30 30 5                                                              (commercial) 50 53 53 12                                                        100 55 55 7                                                                    200 65 65 32                                                                  83-01 25 60 7 20                                                                50 63 20 20                                                                    100 65 43 33                                                                   200 80 70 48                                                                  83-02 25 25 7 5                                                                 50 42 12 25                                                                    100 60 30 22                                                                   200 68 68 50                                                                  83-03 25 22 5 10                                                                50 55 7 33                                                                     100 62 25 27                                                                   200 65 55 48                                                                  83-04 25 57 7 13                                                                50 67 10 32                                                                    100 67 35 32                                                                   200 70 70 45                                                                  83-05 25 30 3 15                                                                50 47 27 27                                                                    100 55 42 37                                                                   200 65 60 38                                                                  83-06 25 28 0 3                                                                 50 50 0 10                                                                     100 55 30 25                                                                   200 67 58 47                                                                  83-07 25 35 20 17                                                               50 55 35 27                                                                    100 58 63 32                                                                   200 67 67 55                                                                  83-08 25 40 20 8                                                                50 57 30 28                                                                    100 60 60 30                                                                   200 70 77 48                                                                  83-09 25 47 20 22                                                               50 55 35 35                                                                    100 62 65 38                                                                   200 68 82 50                                                                  83-10 25 28 0 5                                                                 50 48 0 10                                                                     100 53 5 25                                                                    200 62 35 40                                                                  83-11 25 35 0 5                                                                 50 43 0 30                                                                     100 50 0 35                                                                    200 65 43 47                                                                  83-12 25 40 5 5                                                                 50 55 18 35                                                                    100 60 47 38                                                                   200 70 62 48                                                                ______________________________________                                    

Results of this test using acifluorfen as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (83-03) gave effectiveness similar to that obtained with the lecithin-based adjuvant LI-700 (83-06) widely used in the art.

Butyl stearate at 0.05% alone (83-05) and in combination with lecithin (83-02) enhanced effectiveness, particularly on ECHCF.

Fluorad FC-754, either alone (83-04) or in combination with lecithin (83-01) gave effectiveness on ABUTH and SIDSP superior to that obtained with the commercial standard.

Oleth-20 at the low concentration of 0.05% (83-09) gave effectiveness superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (83-07) or 0.01% methyl oleate (83-08) did not provide further enhancement.

Example 84

Spray compositions were prepared containing asulam and excipient ingredients. Compositions 84-01 to 84-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 11 days after planting ECHCF and 21 days after planting SIDSP. Evaluation of herbicidal inhibition was done 14 days after application.

Standards included technical asulam and Asulox, a commercial formulation of asulam from Rhone-Poulenc. Results, averaged for all replicates of each treatment, are shown in Table 84.

                  TABLE 84                                                         ______________________________________                                                     Asulam rate                                                                              % Inhibition                                             Spray composition                                                                          g a.i./ha ABUTH     ECHCF SIDSP                                    ______________________________________                                         Asulam      200       0         12    0                                          (technical) 400 17 27 5                                                         800 48 32 20                                                                   1400 42 50 37                                                                 Asulox 200 3 5 0                                                               (commercial) 400 27 30 20                                                       800 52 45 25                                                                   1400 50 60 40                                                                 84-01 200 5 8 13                                                                400 23 45 22                                                                   800 50 50 30                                                                   1400 60 65 48                                                                 84-02 200 0 20 17                                                               400 33 40 20                                                                   800 47 48 33                                                                   1400 53 68 55                                                                 84-03 200 3 20 3                                                                400 28 52 7                                                                    800 50 50 23                                                                   1400 50 58 43                                                                 84-04 200 3 40 7                                                                400 35 45 18                                                                   800 52 50 25                                                                   1400 58 60 42                                                                 84-05 200 0 10 3                                                                400 23 30 18                                                                   800 33 50 32                                                                   1400 45 57 38                                                                 84-06 200 2 30 10                                                               400 8 47 17                                                                    800 50 55 28                                                                   1400 52 63 40                                                                 84-07 200 0 43 3                                                                400 22 48 17                                                                   800 40 55 28                                                                   1400 52 60 33                                                                 84-08 200 7 47 22                                                               400 20 48 22                                                                   800 53 55 30                                                                   1400 57 60 33                                                                 84-09 200 0 45 7                                                                400 25 50 7                                                                    800 53 60 32                                                                   1400 55 63 37                                                                 84-10 200 22 37 10                                                              400 27 45 10                                                                   800 50 43 23                                                                   1400 52 52 27                                                                 84-11 200 25 33 5                                                               400 15 37 13                                                                   800 48 42 25                                                                   1400 42 52 28                                                                 84-12 200 3 25 17                                                               400 13 42 18                                                                   800 50 45 30                                                                   1400 52 50 33                                                               ______________________________________                                    

Results of this test using asulam as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (84-03) gave similar enhancement to that obtained with the lecithin-based adjuvant LI-700 (84-06) widely used in the art.

Butyl stearate alone at 0.05% (84-05) enhanced effectiveness on ECHCF.

The combination of lecithin and butyl stearate (84-02) gave greater enhancement of effectiveness than either excipient substance alone.

Fluorad FC-754, either alone (84-04) or in combination with lecithin (84-01) gave effectiveness equal to that obtained with the commercial standard.

Oleth-20 at the low concentration of 0.05% (84-09) gave, at low exogenous chemical rates, effectiveness on ECHCF superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (84-07) or 0.01% methyl oleate (84-08) did not provide further enhancement.

Example 85

Spray compositions were prepared containing dicamba sodium salt and excipient ingredients. Compositions 85-01 to 85-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 8 days after planting ECHCF and 21 days after planting SIDSP. Evaluation of herbicidal inhibition was done 17 days after application.

Standards included technical dicamba sodium and Banvel, a commercial formulation of dicamba from Sandoz. Results, averaged for all replicates of each treatment, are shown in Table 85.

                  TABLE 85                                                         ______________________________________                                                     Dicamba rate                                                                             % Inhibition                                             Spray composition                                                                          g a.i./ha ABUTH     ECHCF SIDSP                                    ______________________________________                                         Dicamba     25        47        0     30                                         (technical) 50 63 0 40                                                          100 82 0 50                                                                    200 93 5 58                                                                   Banvel 25 47 0 35                                                              (commercial) 50 68 0 40                                                         100 91 0 53                                                                    200 93 3 63                                                                   85-01 25 42 0 38                                                                50 67 0 48                                                                     100 92 0 67                                                                    200 93 3 73                                                                   85-02 25 43 0 43                                                                50 58 0 50                                                                     100 85 0 62                                                                    200 89 8 72                                                                   85-03 25 50 0 32                                                                50 65 0 45                                                                     100 90 0 60                                                                    200 94 13 68                                                                  85-04 25 43 0 35                                                                50 65 0 42                                                                     100 94 0 53                                                                    200 94 13 67                                                                  85-05 25 50 0 35                                                                50 68 0 40                                                                     100 88 0 53                                                                    200 92 15 60                                                                  85-06 25 40 0 40                                                                50 65 0 45                                                                     100 88 0 52                                                                    200 92 8 70                                                                   85-07 25 45 0 42                                                                50 57 0 45                                                                     100 88 0 62                                                                    200 88 20 68                                                                  85-08 25 40 0 38                                                                50 62 0 45                                                                     100 97 18 62                                                                   200 93 17 73                                                                  85-09 25 33 0 35                                                                50 60 0 45                                                                     100 93 0 63                                                                    200 96 15 73                                                                  85-10 25 35 0 30                                                                50 57 0 43                                                                     100 90 0 50                                                                    200 90 3 70                                                                   85-11 25 45 0 30                                                                50 53 0 42                                                                     100 89 0 55                                                                    200 92 0 73                                                                   85-12 25 38 0 37                                                                50 60 0 45                                                                     100 96 0 52                                                                    200 93 0 70                                                                 ______________________________________                                    

Results of this test using paraquat as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (85-03) gave similar enhancement of effectiveness to that obtained with the lecithin-based adjuvant LI-700 (85-06) widely used in the art.

Butyl stearate alone at 0.05% (85-05) provided slight enhancement of effectiveness.

The combination of lecithin and butyl stearate (85-02) gave greater enhancement of effectiveness on SIDSP than either of these two excipient substances alone.

Fluorad FC-754 (85-04) provided effectiveness similar to that obtained with the commercial standard. Further enhancement on SIDSP was obtained with the combination of Fluorad FC-754 and lecithin (85-01).

Oleth-20 at the low concentration of 0.05% (85-09) gave, effectiveness on SIDSP superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (85-07) or 0.01% methyl oleate (85-08) did not provide further enhancement.

Example 86

Spray compositions were prepared containing metsulfuron-methyl and excipient ingredients. Compositions 86-01 to 86-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 8 days after planting ECHCF and 21 days after planting SIDSP. Evaluation of herbicidal inhibition was done 14 days after application.

Standards included technical metsulfuron-methyl and Ally, a commercial formulation of metsulfuron from DuPont. Results, averaged for all replicates of each treatment, are shown in Table 86.

                  TABLE 86                                                         ______________________________________                                                    Metsulfuron rate                                                                           % Inhibition                                            Spray composition                                                                         g a.i./ha   ABUTH    ECHCF SIDSP                                    ______________________________________                                         Metsulfuron                                                                               0.5         72       0      5                                         (technical) 1 90 0 23                                                           5 96 0 50                                                                      10 97 30 55                                                                   Ally 0.5 75 0 5                                                                (commercial) 1 85 0 22                                                          5 95 0 42                                                                      10 97 25 53                                                                   86-01 0.5 95 0 47                                                               1 96 20 53                                                                     5 97 25 62                                                                     10 98 45 62                                                                   86-02 0.5 87 0 40                                                               1 90 10 55                                                                     5 95 10 58                                                                     10 96 40 63                                                                   86-03 0.5 87 0 27                                                               1 90 0 40                                                                      5 96 10 57                                                                     10 97 33 63                                                                   86-04 0.5 90 0 33                                                               1 95 10 50                                                                     5 98 17 62                                                                     10 99 28 58                                                                   86-05 0.5 85 0 27                                                               1 90 0 33                                                                      5 95 0 47                                                                      10 95 13 60                                                                   86-06 0.5 77 0 30                                                               1 89 10 47                                                                     5 96 17 62                                                                     10 98 33 60                                                                   86-07 0.5 94 0 55                                                               1 97 10 60                                                                     5 98 43 60                                                                     10 97 55 65                                                                   86-08 0.5 93 0 55                                                               1 96 5 58                                                                      5 97 42 60                                                                     10 97 50 60                                                                   86-09 0.5 93 0 55                                                               1 97 10 62                                                                     5 98 55 62                                                                     10 98 65 63                                                                   86-10 0.5 85 0 28                                                               1 82 0 30                                                                      5 95 10 52                                                                     10 96 17 57                                                                   86-11 0.5 73 0 25                                                               1 88 20 28                                                                     5 94 25 53                                                                     10 96 32 57                                                                   86-12 0.5 75 0 32                                                               1 85 20 37                                                                     5 94 23 55                                                                     10 96 25 57                                                                 ______________________________________                                    

Results of this test using metsulfuron as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospolipid (86-03) was slightly more effective excipient than the lecithin-based adjuvant LI-700 (86-06) widely used in the art in improving perfromance on ABUTH at the lowest exogenous chemical rate tested.

Butyl stearate alone at 0.05% (86-05) enhanced effectiveness to a level superior to that obtained with the commercial standard.

The combination of lecithin and butyl stearate (86-02) gave greater enhancement of effectiveness than was obtained with either of these two excipient substances alone.

Fluorad FC-754, either alone (86-04) or in combination with lecithin (86-01) gave high effectiveness, superior to that obtained with the commercial standard.

Oleth-20 at the low concentration of 0.05% (86-09) gave high effectiveness, superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (86-07) or 0.01% methyl oleate (86-08) did not provide further enhancement.

Example 87

Spray compositions were prepared containing imazethapyr and excipient ingredients. Compositions 87-01 to 87-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 14 days after planting ECHCF and 21 days after planting SIDSP. Evaluation of herbicidal inhibition was done 14 days after application.

Standards included technical imazethapyr and Pursuit, a commercial formulation of imazethapyr from American Cyanamid. Results, averaged for all replicates of each treatment, are shown in Table 87.

                  TABLE 87                                                         ______________________________________                                                    Imazethapyr rate                                                                           % Inhibition                                            Spray composition                                                                         g a.i./ha   ABUTH    ECHCF SIDSP                                    ______________________________________                                         Imazethapyr                                                                               5           78       5     20                                         (technical) 10 83 20 30                                                         25 93 35 40                                                                    50 94 53 50                                                                   Pursuit 5 70 5 25                                                              (commercial) 10 73 33 30                                                        25 90 50 42                                                                    50 93 62 57                                                                   87-01 5 70 45 35                                                                10 75 62 52                                                                    25 92 63 57                                                                    50 93 72 62                                                                   87-02 5 73 57 32                                                                10 75 67 43                                                                    25 90 70 52                                                                    50 92 72 57                                                                   87-03 5 70 42 27                                                                10 78 42 35                                                                    25 90 53 45                                                                    50 92 62 52                                                                   87-04 5 73 55 33                                                                10 77 68 45                                                                    25 93 68 47                                                                    50 94 68 60                                                                   87-05 5 73 47 32                                                                10 73 45 40                                                                    25 90 62 47                                                                    50 91 68 52                                                                   87-06 5 78 72 30                                                                10 83 70 35                                                                    25 93 77 62                                                                    50 94 78 58                                                                   87-07 5 82 75 38                                                                10 90 90 52                                                                    25 93 93 53                                                                    50 97 97 62                                                                   87-08 5 75 77 38                                                                10 90 92 50                                                                    25 95 93 57                                                                    50 97 99 63                                                                   87-09 5 78 80 40                                                                10 83 89 63                                                                    25 93 93 62                                                                    50 96 93 60                                                                   87-10 5 85 50 37                                                                10 77 50 45                                                                    25 91 63 48                                                                    50 93 75 57                                                                   87-11 5 75 38 43                                                                10 80 38 37                                                                    25 92 62 45                                                                    50 93 73 53                                                                   87-12 5 75 55 38                                                                10 83 60 43                                                                    25 92 67 53                                                                    50 93 77 55                                                                 ______________________________________                                    

Results of this test using imazethapyr as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (87-03) was a less effective excipient than the lecithin-based adjuvant LI-700 (87-06).

Butyl stearate alone at 0.05% (87-05) significantly enhanced effectiveness on ECHCF and slightly on SIDSP.

The combination of lecithin and butyl stearate (87-02) gave enhancement of effectiveness on ECHCF greater than that obtained with either of these two excipient substances alone.

Fluorad FC-754 (87-04) gave effectiveness on ECHCF superior to that obtained with the commercial standard. The combination of Fluorad FC-754 and lecithin (87-01) provided slight further enhancement of effectiveness on SIDSP.

Oleth-20 at the low concentration of 0.05% (87-09) gave extremely high effectiveness, greatly superior to that obtained with the commercial standard, especially on ECHCF. Addition of 0.005% butyl stearate (87-07) further enhanced performance of low exogenous chemical rates on ABUTH more effectively than addition of 0.01% methyl oleate (87-08).

Example 88

Spray compositions were prepared containing fluazifop-p-butyl salt and excipient ingredients. Compositions 88-01 to 88-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and broadleaf signalgrass (Brachiaria platyphylla, BRAPP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 15 days after planting ABUTH, 15 days after planting ECHCF and 16 days after planting BRAPP. Evaluation of herbicidal inhibition was done 10 days after application.

Standards included technical fluazifop-p-butyl and Fusilade 5, a commercial formulation of fluazifop-p-butyl from Zeneca. Results, averaged for all replicates of each treatment, are shown in Table 88.

                  TABLE 88                                                         ______________________________________                                                    Fluazifop-p rate                                                                           % Inhibition                                            Spray composition                                                                         g a.i./ha   ABUTH    ECHCF BRAPP                                    ______________________________________                                         Fluazifop-p-butyl                                                                         2           0        0     20                                         (technical) 5 0 3 35                                                            15 5 45 65                                                                     30 5 57 78                                                                    Fusilade 5 2 0 0 27                                                            (commercial) 5 0 27 33                                                          15 5 52 78                                                                     30 7 75 85                                                                    88-01 2 0 0 20                                                                  5 2 27 30                                                                      15 5 58 78                                                                     30 10 87 83                                                                   88-02 2 0 7 25                                                                  5 0 35 30                                                                      15 2 58 75                                                                     30 8 78 75                                                                    88-03 2 0 0 18                                                                  5 0 8 27                                                                       15 0 45 75                                                                     30 0 55 75                                                                    88-04 2 0 20 32                                                                 5 2 42 25                                                                      15 2 55 72                                                                     30 5 80 78                                                                    88-05 2 0 13 32                                                                 5 2 42 32                                                                      15 2 55 72                                                                     30 7 58 73                                                                    88-06 2 2 17 23                                                                 5 0 20 25                                                                      15 0 50 75                                                                     30 0 73 77                                                                    88-07 2 0 50 40                                                                 5 0 52 60                                                                      15 0 67 80                                                                     30 0 92 85                                                                    88-08 2 0 43 35                                                                 5 0 55 37                                                                      15 7 88 82                                                                     30 3 96 85                                                                    88-09 2 0 47 18                                                                 5 0 50 35                                                                      15 0 80 80                                                                     30 3 93 85                                                                    88-10 2 0 23 10                                                                 5 0 37 42                                                                      15 5 55 75                                                                     30 10 58 80                                                                   88-11 2 0 7 10                                                                  5 0 30 28                                                                      15 0 50 62                                                                     30 12 53 68                                                                   88-12 2 0 5 20                                                                  5 0 7 35                                                                       15 5 48 68                                                                     30 12 60 77                                                                 ______________________________________                                    

Results of this test using fluazifop-p-butyl as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (88-03) was a less effective excipient on ECHCF than the lecithin-based adjuvant LI-700 (88-06).

Butyl stearate alone at 0.05% (88-05) and in combination with lecithin (88-02) enhanced effectiveness, especially on ECHCF.

Fluorad FC-754, either alone (88-04) or in combination with lecithin (88-01) gave effectiveness equal or superior to that obtained with the commercial standard.

Oleth-20 at the low concentration of 0.05% (88-09) gave extremely high effectiveness on ECHCF, superior to that obtained with the commercial standard. Addition of 0.005% butyl stearate (88-07) or 0.01% methyl oleate (88-08) did not provide significant further enhancement.

Example 89

Spray compositions were prepared containing alachlor and excipient ingredients. Compositions 89-01 to 89-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 8 days after planting ECHCF and 14 days after planting SIDSP. Evaluation of herbicidal inhibition was done 9 days after application.

Standards included technical alachlor and Lasso, a commercial formulation of alachlor from Monsanto Company. Results, averaged for all replicates of each treatment, are shown in Table 89.

                  TABLE 89                                                         ______________________________________                                                    Alachlor rate                                                                              % Inhibition                                            Spray composition                                                                         g a.i./ha   ABUTH    ECHCF SIDSP                                    ______________________________________                                         Alachlor   500         0        0     0                                          (technical) 1000 0 0 0                                                          2000 0 0 0                                                                     4000 0 0 0                                                                    Lasso 500 0 0 0                                                                (commercial) 1000 0 5 13                                                        2000 0 30 17                                                                   4000 15 43 65                                                                 89-01 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 10 0 7                                                                   89-02 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 22 7                                                                    4000 12 47 12                                                                 89-03 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 10 0 0                                                                   89-04 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 5 0 15                                                                   89-05 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 3 0 5                                                                    89-06 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 13 7                                                                    4000 0 37 12                                                                  89-07 500 0 0 0                                                                 1000 0 8 0                                                                     2000 0 28 15                                                                   4000 12 50 20                                                                 89-08 500 0 0 0                                                                 1000 0 8 0                                                                     2000 0 8 0                                                                     4000 5 20 5                                                                   89-09 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 3 0                                                                     4000 12 42 32                                                                 89-10 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 0 0 0                                                                    89-11 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 0 0 0                                                                    89-12 500 0 0 0                                                                 1000 0 0 0                                                                     2000 0 0 0                                                                     4000 0 0 0                                                                  ______________________________________                                    

None of the compositions tested enhanced post-emergence foliar-applied herbicidal effectiveness of alachlor in this test. Alachlor is not known as a foliar-applied herbicide.

Example 90

Spray compositions were prepared containing glufosinate ammonium salt and excipient ingredients. Compositions 90-01 to 90-12 were exactly like compositions 81-01 to 81-12 respectively except that a different active ingredient was used and a range of active ingredient concentrations was selected appropriate to the active ingredient being applied.

Velvetleaf (Abutilon theophrasti, ABUTH), Japanese millet (Echinochloa crus-galli, ECHCF) and prickly sida (Sida spinosa, SIDSP) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 14 days after planting ABUTH, 10 days after planting ECHCF and 17 days after planting SIDSP. Evaluation of herbicidal inhibition was done 11 days after application.

Standard included technical glufosinate ammonium and Liberty, a commercial formulation of glufosinate from AgrEvo. Results, averaged for all replicates of each treatment, are shown in Table 90.

                  TABLE 90                                                         ______________________________________                                                    Glufosinate rate                                                                           % Inhibition                                            Spray composition                                                                         g a.i./ha   ABUTH    ECHCF SIDSP                                    ______________________________________                                         Glufosinate                                                                               50          0        0     5                                          (technical) 100 47 0 10                                                         300 90 23 96                                                                   600 98 43 94                                                                  Liberty 50 77 70 20                                                            (commercial) 100 88 96 93                                                       300 98 100 97                                                                  600 99 100 99                                                                 90-01 50 77 33 70                                                               100 95 58 93                                                                   300 98 95 97                                                                   600 99 99 98                                                                  90-02 50 33 30 50                                                               100 63 32 93                                                                   300 96 52 90                                                                   600 98 96 97                                                                  90-03 50 15 30 38                                                               100 50 33 87                                                                   300 92 40 94                                                                   600 98 70 98                                                                  90-04 50 92 47 50                                                               100 90 53 85                                                                   300 98 98 96                                                                   600 98 99 98                                                                  90-05 50 35 20 20                                                               100 37 30 20                                                                   300 97 45 78                                                                   600 91 53 92                                                                  90-06 50 10 0 20                                                                100 20 3 20                                                                    300 89 47 82                                                                   600 91 94 89                                                                  90-07 50 50 35 70                                                               100 73 52 80                                                                   300 95 87 98                                                                   600 98 98 97                                                                  90-08 50 48 30 88                                                               100 83 50 93                                                                   300 98 97 96                                                                   600 98 99 96                                                                  90-09 50 58 35 92                                                               100 91 62 93                                                                   300 98 96 97                                                                   600 98 99 96                                                                  90-10 50 30 30 0                                                                100 43 35 10                                                                   300 96 43 92                                                                   600 95 70 91                                                                  90-11 50 33 35 0                                                                100 53 35 7                                                                    300 96 43 89                                                                   600 97 88 93                                                                  90-12 50 37 5 5                                                                 100 37 20 10                                                                   300 95 40 88                                                                   600 97 85 93                                                                ______________________________________                                    

Results of this test using glufosinate as the exogenous chemical are summarized as follows:

At the low concentration of 0.05% used here, soybean lecithin containing 45% phospholipid (90-03) was a much more effective excipient than the lecithin-based adjuvant LI-700 (90-06) widely used in the art.

Butyl stearate alone at 0.05% (90-05) enhanced effectiveness on ECHCF.

The combination of lecithin and butyl stearate (90-02) gave greater enhancement of effectiveness than either of these two excipient substances alone.

Fluorad FC-754, either alone (90-04) or in combination with lecithin (90-01) gave extremely high effectiveness, similar to that obtained with the commercial standard.

Oleth-20 at the low concentration of 0.05% (90-09) gave extremely high effectiveness, superior on SIDSP to that obtained with the commercial standard.

Addition of 0.005% butyl stearate (90-07) or 0.01% methyl oleate (90-08) did not provide further enhancement.

Example 91

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 91a. Concentrate compositions 91-01 to 91-12 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix). Concentrate compositions 91-13 to 91-18 contained colloidal particulates but no surfactant.

The colloidal particulates of this example were in general too large to confer good storage stability to the compositions tested.

                  TABLE 91a                                                        ______________________________________                                         Glypho-                                                                        Concentrate                                                                            sate    % w/w        Type of Type of                                   composition                                                                            g a.e./l                                                                               Surfactant                                                                              Silica                                                                               surfactant                                                                             silica                                  ______________________________________                                         91-01   488     3.0      0.8   steareth-20                                                                            Sident 9                                  91-02 488 3.0 0.8 steareth-20 Sipernat 22                                      91-03 488 3.0 0.8 steareth-20 Sipernat 22S                                     91-04 488 3.0 0.8 oleth-20 Sident 9                                            91-05 488 3.0 0.8 oleth-20 Sipernat 22                                         91-06 488 3.0 0.8 oleth-20 Sipernat 22S                                        91-07 488 3.0 1.5 steareth-20 Sident 9                                         91-08 488 3.0 1.5 steareth-20 Sipernat 22                                      91-09 488 3.0 1.5 steareth-20 Sipernat 22S                                     91-10 488 3.0 1.5 oleth-20 Sident 9                                            91-11 488 3.0 1.5 oleth-20 Sipernat 22                                         91-12 488 3.0 1.5 oleth-20 Sipernat 22S                                        91-13 488  0.8 none Sident 9                                                   91-14 488  1.5 none Sipernat 22                                                91-15 488  0.8 none Sipernat 22S                                               91-16 488  1.5 none Sident 9                                                   91-17 488  0.8 none Sipernat 22                                                91-18 488  1.5 none Sipernat 22S                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 21 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 14 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 91B.

                  TABLE 91b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          3        37                                            200 10 57                                                                      300 43 87                                                                      400 57 88                                                                     Formulation J 100 33 80                                                         200 72 98                                                                      300 96 99                                                                      400 97 99                                                                     91-01 100 47 89                                                                 200 78 97                                                                      300 87 99                                                                      400 98 99                                                                     91-02 100 37 83                                                                 200 70 99                                                                      300 90 99                                                                      400 95 100                                                                    91-03 100 40 89                                                                 200 70 99                                                                      300 90 100                                                                     400 95 100                                                                    91-04 100 37 94                                                                 200 58 98                                                                      300 87 99                                                                      400 95 100                                                                    91-05 100 30 60                                                                 200 73 95                                                                      300 85 99                                                                      400 97 99                                                                     91-06 100 33 67                                                                 200 70 97                                                                      300 78 99                                                                      400 92 100                                                                    91-07 100 32 81                                                                 200 60 99                                                                      300 83 98                                                                      400 88 100                                                                    91-08 100 40 63                                                                 200 65 93                                                                      300 90 99                                                                      400 90 100                                                                    91-09 100 43 70                                                                 200 55 98                                                                      300 88 99                                                                      400 94 100                                                                    91-10 100 33 91                                                                 200 70 99                                                                      300 83 99                                                                      400 94 99                                                                     91-11 100 20 63                                                                 200 70 97                                                                      300 92 100                                                                     400 94 100                                                                    91-12 100 48 67                                                                 200 70 93                                                                      300 88 98                                                                      400 94 100                                                                    91-13 100 20 50                                                                 200 60 83                                                                      300 83 97                                                                      400 94 99                                                                     91-14 100 43 43                                                                 200 67 88                                                                      300 83 97                                                                      400 91 99                                                                     91-15 100 30 50                                                                 200 67 73                                                                      300 77 96                                                                      400 97 96                                                                     91-16 100 43 43                                                                 200 75 79                                                                      300 87 94                                                                      400 87 91                                                                     91-17 100 40 27                                                                 200 68 53                                                                      300 87 92                                                                      400 93 98                                                                     91-18 100 47 10                                                                 200 75 37                                                                      300 83 63                                                                      400 92 88                                                                   ______________________________________                                    

Many of the high-load (488 g a.e./l) glyphosate formulations of this Example exhibited herbicidal effectiveness equal to or greater than that obtained with commercial standard Formulation J, in spite of containing only 3% alkylether surfactant.

Example 92

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 92a. Concentrate compositions 92-01 to 92-12 and 92-14 to 92-16 are oil-in-water emulsions and were prepared by process (vii). Concentrate composition 92-13 is an aqueous solution concentrate and was prepared by process (viii).

                  TABLE 92a                                                        ______________________________________                                                 Glypho- % w/w                                                          Concentrate                                                                            sate           Surfac-                                                                              Type of  Type of                                    composition g a.e./l Oil tant oil surfactant                                 ______________________________________                                         92-01   163     0.5    5.0   butyl stearate                                                                          steareth-30                                92-02 163 0.5 5.0 methyl stearate steareth-30                                  92-03 163 0.5 5.0 butyl stearate Neodol 45-13                                  92-04 163 0.5 5.0 methyl stearate Neodol 45-13                                 92-05 163 0.5 5.0 butyl stearate ceteareth-15                                  92-06 163 0.5 5.0 methyl stearate ceteareth-15                                 92-07 163 0.5 5.0 butyl stearate laureth-23                                    92-08 163 0.5 5.0 butyl stearate oleth-20                                      92-09 163 0.5 5.0 butyl stearate steareth-20                                   92-10 163 0.5 5.0 butyl stearate ceteareth-27                                  92-11 163 0.3 5.0 butyl stearate ceteareth-27                                  92-12 163 0.3 2.5 butyl stearate ceteareth-27                                  92-13 163  5.0 none ceteareth-27                                               92-14 163 0.5 5.0 methyl stearate ceteareth-27                                 92-15 163 0.5 5.0 methyl stearate steareth-20                                  92-16 163 0.5 5.0 methyl stearate oleth-20                                   ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 20 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 92b.

                  TABLE 92b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         45        57                                            200 35 53                                                                      300 50 57                                                                      400 38 33                                                                     Formulation C 100 70 98                                                         200 90 99                                                                      300 97 100                                                                     400 100 100                                                                   Formulation J 100 72 88                                                         200 93 99                                                                      300 97 99                                                                      400 98 99                                                                     92-01 100 83 97                                                                 200 97 100                                                                     300 99 100                                                                     400 100 100                                                                   92-02 100 80 99                                                                 200 96 100                                                                     300 99 100                                                                     400 99 100                                                                    92-03 100 73 98                                                                 200 92 100                                                                     300 98 99                                                                      400 99 100                                                                    92-04 100 73 98                                                                 200 87 99                                                                      300 97 99                                                                      400 99 100                                                                    92-05 100 80 98                                                                 200 87 100                                                                     300 98 100                                                                     400 100 100                                                                   92-06 100 78 97                                                                 200 95 98                                                                      300 98 100                                                                     400 99 100                                                                    92-07 100 78 98                                                                 200 88 100                                                                     300 96 100                                                                     400 98 100                                                                    92-08 100 75 98                                                                 200 93 99                                                                      300 97 99                                                                      400 100 99                                                                    92-09 100 83 93                                                                 200 95 100                                                                     300 98 100                                                                     400 100 100                                                                   92-10 100 80 97                                                                 200 95 98                                                                      300 98 99                                                                      400 100 100                                                                   92-11 100 80 97                                                                 200 93 99                                                                      300 98 100                                                                     400 100 99                                                                    92-12 100 77 93                                                                 200 88 100                                                                     300 99 100                                                                     400 99 100                                                                    92-13 100 80 73                                                                 200 95 95                                                                      300 99 100                                                                     400 100 100                                                                   92-14 100 77 94                                                                 200 92 99                                                                      300 98 100                                                                     400 100 99                                                                    92-15 100 78 92                                                                 200 94 99                                                                      300 98 100                                                                     400 99 100                                                                    92-16 100 77 93                                                                 200 90 98                                                                      300 98 99                                                                      400 99 100                                                                  ______________________________________                                    

Extremely high herbicidal effectiveness was provided by ceteareth-27 (composition 92-13); this was further enhanced by addition of a small amount of butyl stearate (92-10, 92-11) or methyl stearate (92-14). Compositions performing better than commercial standard Formulations C and J, at least on ABUTH, included those containing steareth-30, steareth-20 or ceteareth-27; in this test oleth-20 was not quite as effective as these saturated alkylethers.

Example 93

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 93a. All are oil-in-water emulsions and were prepared by process (vii). Lecithin (45% phospholipid, Avanti) was first dispersed in water using sonication.

                  TABLE 93a                                                        ______________________________________                                         Concen-                                                                          trate Glypho- % w/w                                                          compo-                                                                               sate            Butyl Ethomeen                                                                              Ceteareth-                                                                            Ceteareth-                             sition g a.e./l Lecithin stearate T/25 20 27                                 ______________________________________                                         93-01 220     0.75    0.75  1.5                                                  93-02 220 0.75 0.75 1.5                                                        93-03 220 0.75 0.75 3.0                                                        93-04 220 0.75 7.50 1.5                                                        93-05 220 0.75 7.50 3.0                                                        93-06 220 3.75 3.75 3.0                                                        93-07 220 1.50 1.50 3.0                                                        93-08 220 1.50 1.50 1.5                                                        93-09 220 3.75 3.75 1.5 1.5                                                    93-10 220 1.50 1.50 1.5 1.5                                                    93-11 220 3.75 7.50 1.5 1.5                                                    93-12 220 3.75 1.50 1.5 1.5                                                    93-13 220 0.75 3.75 1.5  1.5                                                   93-14 220 0.75 7.50 1.5  1.5                                                   93-15 220 0.75 3.75 3.0  3.0                                                   93-16 220 0.75 7.50 3.0  3.0                                                   93-17 220  7.50 3.0                                                            93-18 220 0.75 7.50   3.0                                                    ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 23 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 93b.

                  TABLE 93b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         12        62                                            200 5 55                                                                       300 23 63                                                                      400 43 78                                                                     Formulation J 100 27 82                                                         200 62 98                                                                      300 88 95                                                                      400 96 99                                                                     93-01 100 13 79                                                                 200 68 95                                                                      300 82 99                                                                      400 95 91                                                                     93-02 100 27 82                                                                 200 60 97                                                                      300 81 95                                                                      400 87 99                                                                     93-03 100 37 77                                                                 200 62 96                                                                      300 78 98                                                                      400 89 90                                                                     93-04 100 37 84                                                                 200 57 95                                                                      300 84 99                                                                      400 89 100                                                                    93-05 100 33 77                                                                 200 65 100                                                                     300 78 97                                                                      400 88 97                                                                     93-06 100 43 78                                                                 200 62 95                                                                      300 87 97                                                                      400 95 96                                                                     93-07 100 48 78                                                                 200 80 91                                                                      300 90 99                                                                      400 76 93                                                                     93-08 100 48 83                                                                 200 67 89                                                                      300 86 96                                                                      400 93 97                                                                     93-09 100 62 84                                                                 200 82 98                                                                      300 85 99                                                                      400 91 97                                                                     93-10 100 63 80                                                                 200 75 96                                                                      300 85 99                                                                      400 99 99                                                                     93-11 100 42 75                                                                 200 78 98                                                                      300 92 99                                                                      400 93 100                                                                    93-12 100 52 80                                                                 200 73 93                                                                      300 86 99                                                                      400 97 97                                                                     93-13 100 55 83                                                                 200 75 97                                                                      300 97 99                                                                      400 92 99                                                                     93-14 100 52 87                                                                 200 73 95                                                                      300 91 97                                                                      400 87 98                                                                     93-15 100 57 83                                                                 200 92 96                                                                      300 98 100                                                                     400 100 98                                                                    93-16 100 79 88                                                                 200 87 97                                                                      300 99 99                                                                      400 97 94                                                                     93-17 100 58 83                                                                 200 47 94                                                                      300 88 98                                                                      400 91 93                                                                     93-18 100 58 87                                                                 200 75 91                                                                      300 83 99                                                                      400 91 98                                                                   ______________________________________                                    

Outstanding herbicidal effectiveness was provided by composition 93-18, containing lecithin, ceteareth-27 and butyl stearate. Addition of 3% Ethomeen T/25 (93-16) further enhanced effectiveness. Slightly reduced effectiveness at the lowest glyphosate rate was observed on ABUTH when the butyl stearate concentration was cut in half (93-15).

Example 94

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 94a. Concentrate compositions 94-01 to 94-04, 94-06, 94-08, 94-10 and 94-18 are oil-in-water emulsions and were prepared by process (vii). Concentrate compositions 94-05, 94-07 and 94-09 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 94-11 to 94-17 contain colloidal particulates and were prepared by process (ix).

The compositions of this example all showed acceptable storage stability. The compositions shown as containing colloidal particulate were not storage-stable unless the colloidal particulate was included as shown.

                  TABLE 94a                                                        ______________________________________                                                     % w/w                                                              Concentrate                                                                            Glyphosate                                                                               Butyl   Surfac-                                                                              Aerosil                                                                              Type of                                    composition g a.e./l stearate tant 380 surfactant                            ______________________________________                                         94-01   163       0.5     5.0         steareth-20                                94-02 163 0.5 5.0  ceteareth-27                                                94-03 163 0.5 5.0  oleth-20                                                    94-04 163 0.5 5.0  ceteth-20                                                   94-05 163  5.0  ceteth-20                                                      94-06 163 0.5 5.0  Neodol 45-13                                                94-07 163  5.0  Neodol 45-13                                                   94-08 163 0.5 5.0  ceteareth-15                                                94-09 163  5.0  ceteareth-15                                                   94-10 163 0.5 5.0  steareth-30                                                 94-11 360 1.0 10.0 1.25 ceteth-20                                              94-12 360 1.0 10.0 1.25 Neodol 45-13                                           94-13 360 1.0 10.0 1.25 ceteareth-15                                           94-14 360 1.0 10.0 1.25 steareth-30                                            94-15 360 1.0 10.0 1.25 steareth-20                                            94-16 360 1.0 10.0 1.25 oleth-20                                               94-17 360 1.0 10.0 1.25 ceteareth-27                                           94-18 163 0.5 5.0  laureth-23                                                ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 22 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 94b.

                  TABLE 94b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         0         30                                            200 2 60                                                                       300 17 75                                                                      400 50 73                                                                     Formulation J 100 20 63                                                         200 42 98                                                                      300 75 100                                                                     400 83 98                                                                     94-01 100 27 57                                                                 200 67 98                                                                      300 80 99                                                                      400 87 98                                                                     94-02 100 27 63                                                                 200 53 87                                                                      300 77 99                                                                      400 87 99                                                                     94-03 100 12 50                                                                 200 53 99                                                                      300 65 100                                                                     400 83 99                                                                     94-04 100 20 63                                                                 200 50 98                                                                      300 73 98                                                                      400 87 98                                                                     94-05 100 18 70                                                                 200 57 93                                                                      300 80 99                                                                      400 83 99                                                                     94-06 100 17 63                                                                 200 35 95                                                                      300 60 100                                                                     400 75 100                                                                    94-07 100 3 43                                                                  200 43 95                                                                      300 62 100                                                                     400 68 96                                                                     94-08 100 20 43                                                                 200 43 88                                                                      300 75 99                                                                      400 80 97                                                                     94-09 100 37 57                                                                 200 55 93                                                                      300 83 100                                                                     400 83 99                                                                     94-10 100 37 50                                                                 200 60 96                                                                      300 83 99                                                                      400 88 99                                                                     94-11 100 8 37                                                                  200 37 93                                                                      300 68 99                                                                      400 70 97                                                                     94-12 100 13 43                                                                 200 40 91                                                                      300 67 100                                                                     400 77 96                                                                     94-13 100 25 40                                                                 200 40 80                                                                      300 62 97                                                                      400 78 98                                                                     94-14 100 23 33                                                                 200 37 86                                                                      300 75 99                                                                      400 78 94                                                                     94-15 100 23 30                                                                 200 43 78                                                                      300 53 93                                                                      400 78 98                                                                     94-16 100 23 37                                                                 200 37 95                                                                      300 63 97                                                                      400 78 95                                                                     94-18 100 18 50                                                                 200 45 88                                                                      300 75 69                                                                      400 73 93                                                                     94-19 100 missing missing                                                       200 missing missing                                                            300 missing missing                                                            400 missing missing                                                         ______________________________________                                    

Compositions exhibiting herbicidal effectiveness greater than that provided by commercial standard Formulation J included 94-01 (steareth-20 plus butyl stearate), 94-09 (ceteareth-15) and 94-10 (steareth-20 plus butyl stearate).

Example 95

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 95a. All are oil-in-water emulsions and were prepared by process (vii).

                  TABLE 95a                                                        ______________________________________                                                       % w/w                                                            Concentrate                                                                             Glyphosate Butyl           Type of                                      composition g a.e./l stearate Surfactant surfactant                          ______________________________________                                         95-01    163        1.00     10.0   laureth-23                                   95-02 163 0.50 5.0 laureth-23                                                  95-03 163 0.25 2.5 laureth-23                                                  95-04 163 1.00 10.0 Neodol 1-9                                                 95-05 163 0.50 5.0 Neodol 1-9                                                  95-06 163 0.25 2.5 Neodol 1-9                                                  95-07 163 1.00 10.0 steareth-10                                                95-08 163 0.50 5.0 steareth-10                                                 95-09 163 0.25 2.5 steareth-10                                                 95-10 163 0.50 5.0 steareth-20                                                 95-11 163 0.25 2.5 steareth-20                                                 95-12 163 0.25 1.0 steareth-20                                                 95-13 163 0.50 5.0 oleth-20                                                    95-14 163 0.25 2.5 oleth-20                                                    95-15 163 0.25 1.0 oleth-20                                                    95-16 163 0.50 5.0 ceteareth-27                                                95-17 163 0.25 2.5 ceteareth-27                                                95-18 163 0.25 1.0 ceteareth-27                                              ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 21 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 95b.

                  TABLE 95b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100         0         42                                            200 0 43                                                                       300 23 50                                                                      400 0 28                                                                      Formulation J 100 0 73                                                          200 57 85                                                                      300 68 93                                                                      400 87 94                                                                     95-01 100 18 75                                                                 200 58 92                                                                      300 85 90                                                                      400 94 95                                                                     95-02 100 3 77                                                                  200 47 90                                                                      300 65 89                                                                      400 87 95                                                                     95-03 100 13 80                                                                 200 53 88                                                                      300 72 98                                                                      400 82 99                                                                     95-04 100 0 0                                                                   200 53 88                                                                      300 67 95                                                                      400 83 95                                                                     95-05 100 2 60                                                                  200 50 83                                                                      300 70 93                                                                      400 85 92                                                                     95-06 100 0 52                                                                  200 55 83                                                                      300 62 96                                                                      400 77 98                                                                     95-07 100 8 70                                                                  200 68 95                                                                      300 91 99                                                                      400 95 100                                                                    95-08 100 10 65                                                                 200 67 99                                                                      300 78 99                                                                      400 93 100                                                                    95-09 100 5 80                                                                  200 52 98                                                                      300 75 100                                                                     400 86 98                                                                     95-10 100 0 65                                                                  200 62 84                                                                      300 58 94                                                                      400 75 100                                                                    95-11 100 5 83                                                                  200 50 99                                                                      300 63 97                                                                      400 87 99                                                                     95-12 100 10 76                                                                 200 60 96                                                                      300 72 100                                                                     400 100 100                                                                   95-13 100 20 85                                                                 200 67 100                                                                     300 91 100                                                                     400 96 98                                                                     95-14 100 23 68                                                                 200 62 89                                                                      300 80 100                                                                     400 99 99                                                                     95-15 100 5 57                                                                  200 55 93                                                                      300 89 95                                                                      400 90 98                                                                     95-16 100 30 68                                                                 200 68 94                                                                      300 83 98                                                                      400 100 100                                                                   95-17 100 43 68                                                                 200 62 99                                                                      300 78 100                                                                     400 100 99                                                                    95-18 100 25 52                                                                 200 53 84                                                                      300 85 94                                                                      400 98 95                                                                   ______________________________________                                    

Compositions having a 1:3 or lower weight/weight ratio of surfactant to glyphosate a.e., yet outperforming commercial standard Formulation J at least on ABUTH in this test, included those containing just 1% alkylether surfactant (ratio about 1:15) together with 0.25% butyl stearate, where the alkylether surfactant was steareth-20 (95-12), oleth-20 (95-15) or ceteareth-27 (95-18).

Example 96

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 96a. All are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix).

The compositions of this example all showed acceptable storage stability. The compositions shown as containing colloidal particulate were not storage-stable unless the colloidal particulate was included as shown.

                                      TABLE 96a                                    __________________________________________________________________________     Conc.                                                                              Glyphosate                                                                           % w/w       Type of                                                                              Type of    Other                                   comp.                                                                              g a.e./l                                                                             Surfactant                                                                          Aerosil                                                                            Other                                                                             surfactant                                                                           Aerosil    component                               __________________________________________________________________________     96-01                                                                              488   3.0 1.5     steareth-20                                                                          MOX-80/380 (1:2)                                     96-02 488 4.5 1.5  steareth-20 380                                             96-03 488 4.5 1.5  steareth-20 MOX-80/380 (1:2)                                96-04 488 4.5 1.5  steareth-20 MOX-80/MOX-170 (1:2)                            96-05 488 6.0 1.5 4.12 steareth-20 380 glycerin                                96-06 488 3.0 1.5  steareth-20 380                                             96-07 488 3.0 1.5 7.12 oleth-20 380 propylene glycol                           96-08 488 3.0 1.5  oleth-20 MOX-80/380 (1:2)                                   96-09 488 4.5 1.5  oleth-20 380                                                96-10 488 4.5 1.5  oleth-20 MOX-80/380 (1:2)                                 __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 21 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 96b.

                  TABLE 96b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          0        25                                            200 35 27                                                                      300 48 28                                                                      400 47 48                                                                     Formulation J 100 50 75                                                         200 80 90                                                                      300 97 96                                                                      400 99 98                                                                     96-01 100 53 33                                                                 200 83 52                                                                      300 98 72                                                                      400 98 79                                                                     96-02 100 43 27                                                                 200 80 57                                                                      300 87 73                                                                      400 96 78                                                                     96-03 100 48 30                                                                 200 81 70                                                                      300 98 78                                                                      400 63 57                                                                     96-04 100 45 32                                                                 200 87 75                                                                      300 97 73                                                                      400 98 83                                                                     96-05 100 38 27                                                                 200 37 23                                                                      300 45 32                                                                      400 35 18                                                                     96-06 100 42 40                                                                 200 78 52                                                                      300 91 72                                                                      400 96 80                                                                     96-07 100 37 43                                                                 200 48 32                                                                      300 73 58                                                                      400 55 28                                                                     96-08 100 43 37                                                                 200 68 57                                                                      300 84 62                                                                      400 89 82                                                                     96-09 100 37 32                                                                 200 83 67                                                                      300 94 82                                                                      400 63 48                                                                     96-10 100 32 40                                                                 200 75 68                                                                      300 90 88                                                                      400 65 63                                                                   ______________________________________                                    

Several high-load (488 g a.e./l) glyphosate compositions exhibited herbicidal effectiveness on ABUTH equal to commercial standard Formulation J, but none was equal to Formulation J on ECHCF in this test.

Example 97

Dry granular concentrate compositions were prepared containing glyphosate ammonium salt and excipient ingredients as shown in Table 97a. The preparation procedure was as follows. Ammonium glyphosate powder was added to a blender. Excipient ingredients were slowly added, together with sufficient water to wet the powder and form a stiff dough. The blender was operated for sufficient time to thoroughly mix all ingredients. The dough was then transferred to extrusion apparatus and was extruded to form granules, which were finally dried in a fluid bed dryer.

                                      TABLE 97a                                    __________________________________________________________________________     % w/w                                 Type of                                  Conc.                                                                              Glyphosate                                                                               Butyl    Colloidal                                                                           Type of   colloidal                                  comp. a.e. Lecithin stearate Surfactant particulate surfactant particula                                           te                                       __________________________________________________________________________     97-01                                                                              68.7          21.0      steareth-20                                          97-02 66.0  2.2 22.0  steareth-20                                              97-03 66.1   24.0  oleth-20                                                    97-04 66.0  2.2 22.0  oleth-20                                                 97-05 67.9 10.0 2.0 10.0  MON 0818                                             97-06 59.2 10.0  20.0 + 2.0  FC-754 + MON 0818                                 97-07 68.0   21.0 0.8 Flomo 1407 Aerosil 90                                    97-08 68.0   21.0 0.8 Flomo 1407 Aluminum oxide C                              97-09 66.1   24.0  ceteth-20                                                   97-10 66.0  2.2 22.0  ceteth-20                                                97-11 71.2   16.1 2.0 ceteth-20 Aerosil 380                                    97-12 71.1   16.3 1.0 ceteth-20 Aerosil blend (*)                              97-13 71.2   16.1 2.0 steareth-20 Aerosil 380                                  97-14 71.2   16.1 1.0 steareth-20 Aerosil blend (*)                            97-15 68.0   20.0 1.9 oleth-20 Aerosil-380                                     97-16 70.8   16.6 1.0 oleth-20 Aerosil blend (*)                             __________________________________________________________________________      (*) Aerosil MOX80 + Aerosil MOX170 (1:1)                                 

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 21 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations J and K were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 97b.

                  TABLE 97b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation J 100         52        80                                            200 90 96                                                                      300 96 100                                                                     400 97 99                                                                     Formulation K 100 33 70                                                         200 67 93                                                                      300 83 99                                                                      400 93 100                                                                    97-01 100 47 60                                                                 200 87 98                                                                      300 97 98                                                                      400 100 98                                                                    97-02 100 47 63                                                                 200 80 94                                                                      300 90 99                                                                      400 98 100                                                                    97-03 100 62 62                                                                 200 83 93                                                                      300 97 96                                                                      400 97 100                                                                    97-04 100 47 57                                                                 200 78 94                                                                      300 87 100                                                                     400 98 100                                                                    97-05 100 25 53                                                                 200 60 88                                                                      300 80 97                                                                      400 83 98                                                                     97-06 100 35 37                                                                 200 65 62                                                                      300 83 83                                                                      400 90 95                                                                     97-07 100 63 55                                                                 200 72 97                                                                      300 83 100                                                                     400 94 100                                                                    97-08 100 30 65                                                                 200 72 94                                                                      300 87 100                                                                     400 92 99                                                                     97-09 100 37 63                                                                 200 77 83                                                                      300 88 99                                                                      400 97 99                                                                     97-10 100 40 55                                                                 200 83 93                                                                      300 94 96                                                                      400 98 99                                                                     97-11 100 42 55                                                                 200 78 94                                                                      300 88 92                                                                      400 94 99                                                                     97-12 100 38 58                                                                 200 78 97                                                                      300 92 97                                                                      400 95 100                                                                    97-13 100 25 50                                                                 200 80 88                                                                      300 96 95                                                                      400 98 98                                                                     97-14 100 50 53                                                                 200 88 92                                                                      300 98 99                                                                      400 99 99                                                                     97-15 100 33 57                                                                 200 75 91                                                                      300 94 97                                                                      400 98 99                                                                     97-16 100 33 55                                                                 200 77 90                                                                      300 88 99                                                                      400 96 100                                                                  ______________________________________                                    

Several dry granular compositions of this Example outperformed commercial standard composition K, at least on ABUTH. They included 97-01 to 97-04 and 97-10 to 97-16, all containing an alkylether surfactant (steareth-20, oleth-20 or ceteth-20).

Example 98

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 98a. All are oil-in-water emulsions and were prepared by process (vii). Soybean lecithin (45% phospholipid, Avanti) was first dispersed in water either by ultrasonication or by use of a microfluidizer as indicated in the column of Table 98a headed "Process".

                                      TABLE 98a                                    __________________________________________________________________________               % w/w                                                                Conc.                                                                              Glyphosate                                                                               Butyl                                                                              Ethomeen                                                                            MON                                                                               Ceteareth-                                                                          Ceteareth-                                                                          Process                                      comp. g a.e./l Lecithin stearate T/25 0818 20 27 (*)                         __________________________________________________________________________     98-01                                                                              220   0.75                                                                               3.75                                                                               3.0          3.0  B                                            98-02 220 0.75 0.75 3.0   3.0 B                                                98-03 220 0.75 3.75 3.0  3.0  B                                                98-04 220 0.75 0.75 3.0  3.0  B                                                98-05 220 6.00 1.50 3.0  3.0  B                                                98-06 220 6.00 1.50 3.0   3.0 B                                                98-07 220 4.00 1.00 3.0  3.0  B                                                98-08 220 4.00 1.00 3.0   3.0 B                                                98-09 220 0.75 3.75 3.0   3.0 A                                                98-10 220 0.75 0.75 3.0   3.0 A                                                98-11 220 0.75 3.75 6.0    B                                                   98-12 220 0.75 3.75   6.0  B                                                   98-13 345 6.00 1.50 4.5 4.5   B                                                98-14 345 6.00 1.50 6.0   3.0 B                                                98-15 345 6.00 1.50 6.0 6.0   B                                                98-16 345 0.50 7.50 12.0      B                                                98-17 345 6.00 1.50 4.5 4.5  3.0 B                                           __________________________________________________________________________      (*) Process:                                                                   A Ultrasonicated                                                               B Microfluidized, 3 cycles                                               

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 19 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 98b.

                  TABLE 98b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 150         45        82                                            250 55 71                                                                      350 80 72                                                                      450 88 77                                                                     Formulation J 150 55 83                                                         250 89 88                                                                      350 97 93                                                                      450 99 93                                                                      550 99 87                                                                     98-01 150 92 83                                                                 250 96 96                                                                      350 99 96                                                                      450 100 86                                                                    98-02 150 85 93                                                                 250 97 78                                                                      350 97 90                                                                      450 99 90                                                                     98-03 150 87 85                                                                 250 98 92                                                                      350 99 95                                                                      450 100 95                                                                    98-04 150 87 89                                                                 250 97 92                                                                      350 99 94                                                                      450 99 91                                                                     98-05 150 87 77                                                                 250 98 89                                                                      350 99 93                                                                      450 99 84                                                                     98-06 150 12 18                                                                 250 96 73                                                                      350 99 85                                                                      450 99 84                                                                     98-07 150 82 89                                                                 250 88 96                                                                      350 96 98                                                                      450 97 97                                                                     98-08 150 88 94                                                                 250 95 90                                                                      350 99 98                                                                      450 99 98                                                                     98-09 150 94 94                                                                 250 95 100                                                                     350 97 99                                                                      450 99 98                                                                     98-10 150 94 94                                                                 250 98 99                                                                      350 99 97                                                                      450 99 96                                                                     98-11 150 83 81                                                                 250 94 88                                                                      350 98 93                                                                      450 99 99                                                                     98-12 150 68 79                                                                 250 95 96                                                                      350 98 100                                                                     450 99 98                                                                     98-13 150 86 98                                                                 250 95 98                                                                      350 99 100                                                                     450 100 98                                                                    98-14 150 85 98                                                                 250 98 98                                                                      350 99 98                                                                      450 100 98                                                                    98-15 150 86 95                                                                 250 97 97                                                                      350 99 95                                                                      450 100 96                                                                    98-16 150 93 94                                                                 250 98 98                                                                      350 99 98                                                                      450 100 97                                                                    98-17 150 95 96                                                                 250 98 100                                                                     350 100 100                                                                    450 100 98                                                                  ______________________________________                                    

Many compositions containing lecithin and butyl stearate outperformed commercial standard Formulation J in this test.

Example 99

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 99a. Concentrate compositions 99-04 and 99-05 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 99-06 to 99-13 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix). Concentrate compositions 99-01 to 99-03 contain colloidal particulate but no surfactant.

The compositions of this example containing colloidal particulate all showed acceptable storage stability. Of those containing steareth-20 but no colloidal particulate, composition 99-04 was acceptable storage-stable but composition 99-05 was not.

                                      TABLE 99a                                    __________________________________________________________________________     Concentrate                                                                          Glyphosate                                                                           % w/w          Type of                                             composition                                                                          g a.e./l                                                                             Steareth-20                                                                          Oleth-20                                                                            Aerosil                                                                            Aerosil                                             __________________________________________________________________________     99-01 484              1.5 MOX-80                                                99-02 484   1.5 380                                                            99-03 484   1.5 MOX-80/MOX-170 (1:1)                                           99-04 484 1.5   none                                                           99-05 484 3.0   none                                                           99-06 484 3.0  1.5 MOX-170                                                     99-07 484 3.0  1.5 380                                                         99-08 484 3.0  1.5 MOX-80/380 (1:1)                                            99-09 484 3.0  1.5 MOX-80/MOX-170 (1:1)                                        99-10 484  3.0 1.5 MOX-80                                                      99-11 484  3.0 1.5 MOX-170                                                     99-12 484  3.0 1.5 380                                                         99-13 484  3.0 1.5 MOX-80/380 (1:1)                                          __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 20 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 99b.

                  TABLE 99b                                                        ______________________________________                                                       Glyphosate rate                                                                            % Inhibition                                         Concentrate composition                                                                      g a.e./ha   ABUTH     ECHCF                                      ______________________________________                                         Formulation B 100          3        38                                            200 28 63                                                                      300 37 75                                                                      400 55 78                                                                     Formulation J 100 23 73                                                         200 43 92                                                                      300 67 96                                                                      400 92 97                                                                     99-01 100 23 60                                                                 200 40 77                                                                      300 65 91                                                                      400 75 92                                                                     99-02 100 18 50                                                                 200 25 53                                                                      300 33 75                                                                      400 67 82                                                                     99-03 100 27 57                                                                 200 35 72                                                                      300 50 86                                                                      400 70 93                                                                     99-04 100 42 67                                                                 200 48 78                                                                      300 78 82                                                                      400 80 85                                                                     99-05 100 28 43                                                                 200 45 77                                                                      300 70 92                                                                      400 80 95                                                                     99-06 100 42 57                                                                 200 70 75                                                                      300 89 87                                                                      400 94 94                                                                     99-07 100 43 68                                                                 200 62 90                                                                      300 88 92                                                                      400 97 92                                                                     99-08 100 53 57                                                                 200 72 87                                                                      300 88 94                                                                      400 92 97                                                                     99-09 100 27 60                                                                 200 62 75                                                                      300 75 92                                                                      400 83 90                                                                     99-10 100 47 43                                                                 200 73 73                                                                      300 82 88                                                                      400 97 93                                                                     99-11 100 48 57                                                                 200 63 75                                                                      300 80 91                                                                      400 89 98                                                                     99-12 100 30 40                                                                 200 42 63                                                                      300 68 75                                                                      400 73 83                                                                     99-13 100 37 40                                                                 200 57 75                                                                      300 73 80                                                                      400 78 94                                                                   ______________________________________                                    

Remarkably strong herbicidal effectiveness was provided by composition 99-05, in spite of its very low surfactant (steareth-20) to glyphosate a.e. ratio of about 1:13. Activity, at least on ABUTH, was further improved to a significant degree by inclusion in the composition of colloidal particulates such as Aerosil MOX-170 (99-06), Aerosil 380 (99-07), a blend of Aerosil MOX-80 and Aerosil 380 (99-08), and a blend of Aerosil MOX-80 and Aerosil MOX-170 (99-09).

Example 100

Aqueous and dry granular concentrate compositions were prepared as shown in Table 100a. Dry granular concentrate compositions 100-01 to 100-11 contain glyphosate ammonium salt, and were prepared by the process described in Example 97.

Aqueous concentrate compositions 100-12 to 100-16 contain glyphosate IPA salt and were prepared by process (v), using soybean lecithin (45% phospholipid, Avanti).

                                      TABLE 100a                                   __________________________________________________________________________               % w/w                               Type of                          Conc.                                                                              Glyphosate                                                                           Glyphosate Butyl     Colloidal                                                                           Type of   colloidal                          comp. g a.e./l a.e. Lecithin stearate Surfactant particulate surfactant                                                    particulate                      __________________________________________________________________________     100-01    68.7            21.0      steareth-20                                  100-02  66.1   24.0  oleth-20                                                  100-03  67.9 10.0   2.0 10.0  MON 0818                                         100-04  59.2 10.0   20.0 + 2.0  FC-754 + MON 0818                              100-05  66.1   24.0  ceteth-20                                                 100-06  71.2   16.1 2.0 steareth-20 Aerosil 380                                100-07  71.2   16.1 2.0 steareth-20 Aerosil blend                              100-08  68.0   20.0 1.9 oleth-20 Aerosil 380                                   100-09  63.5   25.0 2.0 steareth-20 Aerosil blend                              100-10  67.9   20.0 2.0 steareth-20 Aerosil blend                              100-11  72.2   15.0 2.0 steareth-20 Aerosil blend                              100-12 370  4.7   4.7  steareth-20                                             100-13 350  4.9   4.9  ceteareth-27                                            100-14 348  5.0   5.0  ceteareth-15                                            100-15 348  5.0   5.0  oleth-20                                                100-16 351  4.4   5.0  steareth-30                                           __________________________________________________________________________      Aerosil blend: Aerosil MOX80 + Aerosil MOX170 (1:1)                      

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 20 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 16 days after application.

Formulations J and K were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 100b.

                  TABLE 100b                                                       ______________________________________                                                      Glyphosate rate                                                                           % Inhibition                                           Concentrate composition                                                                       g a.e./ha    ABUTH    ECHCF                                     ______________________________________                                         Formulation J  100           0       20                                           200 28 57                                                                      300 58 96                                                                      400 73 99                                                                     Formulation K 100 22 13                                                         200 42 83                                                                      300 48 91                                                                      400 58 95                                                                     100-01 100 28 30                                                                200 48 80                                                                      300 80 97                                                                      400 85 99                                                                     100-02 100 43 52                                                                200 68 80                                                                      300 72 88                                                                      400 86 94                                                                     100-03 100 23 37                                                                200 50 83                                                                      300 75 88                                                                      400 85 96                                                                     100-04 100 50 45                                                                200 73 80                                                                      300 85 92                                                                      400 95 94                                                                     100-05 100 18 45                                                                200 65 83                                                                      300 87 95                                                                      400 94 86                                                                     100-06 100 47 50                                                                200 62 68                                                                      300 82 94                                                                      400 91 87                                                                     100-07 100 50 47                                                                200 60 78                                                                      300 87 87                                                                      400 93 93                                                                     100-08 100 30 55                                                                200 55 77                                                                      300 82 85                                                                      400 88 97                                                                     100-09 100 45 50                                                                200 57 78                                                                      300 83 83                                                                      400 84 89                                                                     100-10 100 42 50                                                                200 57 80                                                                      300 73 91                                                                      400 91 90                                                                     100-11 100 28 48                                                                200 50 75                                                                      300 70 87                                                                      400 82 89                                                                     100-12 100 20 40                                                                200 63 80                                                                      300 67 96                                                                      400 80 88                                                                     100-13 100 27 35                                                                200 50 85                                                                      300 77 90                                                                      400 84 86                                                                     100-14 100 27 25                                                                200 40 70                                                                      300 68 94                                                                      400 89 91                                                                     100-15 100 17 20                                                                200 47 82                                                                      300 58 89                                                                      400 91 95                                                                     100-16 100 22 20                                                                200 41 80                                                                      300 84 89                                                                      400 99 98                                                                   ______________________________________                                    

All compositions of the invention in this study exhibited greater herbicidal effectiveness on both ABUTH and ECHCF, in some cases by a very substantial margin, than commercial standard Formulation K.

Example 101

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 101a. All contain colloidal particulates and were prepared by process (ix).

The compositions of this example all showed acceptable storage stability. The compositions shown as containing colloidal particulate were not storage-stable unless the colloidal particulate was included as shown.

                                      TABLE 101a                                   __________________________________________________________________________               % w/w                                                                Conc.                                                                              Glyphosate    Aerosil                                                                            Type of                                                                               Type of                                             comp. g a.e./l Oil Surfactant 380 oil surfactant                             __________________________________________________________________________     101-01                                                                             360   1.0                                                                               10.0 1.25                                                                               butyl stearate                                                                        oleth-20                                            101-02 360 1.0 10.0 1.25 stearylamine oleth-20                                 101-03 360 1.0 10.0 1.25 stearyl alcohol oleth-20                              101-04 360 1.0 10.0 1.25 docosane oleth-20                                     101-05 360  10.0 1.25 none oleth-20                                            101-06 360 1.0 10.0 1.25 butyl stearate steareth-30                            101-07 360 1.0 10.0 1.25 stearylamine steareth-30                              101-08 360 1.0 10.0 1.25 stearyl alcohol steareth-30                           101-09 360 1.0 10.0 1.25 docosane steareth-30                                  101-10 360  10.0 1.25 none steareth-30                                         101-11 360  5.0 + 5.0 1.25 none oleth-20 + steareth-20                         101-12 360  5.0 + 5.0 1.25 none oleth-20 + steareth-30                         101-13 360  5.0 + 5.0 1.25 none oleth-20 + ceteareth-27                        101-14 360  5.0 + 5.0 1.25 none oleth-20 + ceteareth-15                        101-15 360  5.0 + 5.0 1.25 none steareth-30 + steareth-20                      101-16 360  5.0 + 5.0 1.25 none steareth-30 + ceteareth-27                     101-17 360  5.0 + 5.0 1.25 none steareth-30 + ceteareth-15                     101-18 360  10.0 1.25 none laureth-23                                        __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 101b.

                  TABLE 101b                                                       ______________________________________                                                      Glyphosate rate                                                                           % Inhibition                                           Concentrate composition                                                                       g a.e./ha    ABUTH    ECHCF                                     ______________________________________                                         Formulation B  100           0       60                                           200 15 73                                                                      300 33 88                                                                      400 57 91                                                                     Formulation J 100  5 70                                                         200 37 92                                                                      300 80 99                                                                      400 77 96                                                                     101-01 100 13 88                                                                200 32 85                                                                      300 48 98                                                                      400 90 93                                                                     101-02 100 10 70                                                                200 45 98                                                                      300 72 99                                                                      400 80 98                                                                     101-03 100  3 77                                                                200 25 94                                                                      300 47 98                                                                      400 75 99                                                                     101-04 100  7 67                                                                200 23 94                                                                      300 40 99                                                                      400  7 47                                                                     101-05 100  7 76                                                                200 25 88                                                                      300 45 96                                                                      400 75 97                                                                     101-06 100 12 96                                                                200 30 97                                                                      300 45 98                                                                      400 15 60                                                                     101-07 100  8 83                                                                200 12 97                                                                      300 35 94                                                                      400 50 98                                                                     101-08 100 15 72                                                                200 30 88                                                                      300 40 99                                                                      400  0 33                                                                     101-09 100  5 73                                                                200 15 94                                                                      300 47 99                                                                      400  5 53                                                                     101-10 100  7 79                                                                200 15 95                                                                      300 45 98                                                                      400 62 99                                                                     101-11 100  5 84                                                                200 13 98                                                                      300 30 98                                                                      400 55 100                                                                    101-12 100  3 95                                                                200 17 99                                                                      300 28 99                                                                      400 67 100                                                                    101-13 100  5 90                                                                200 17 99                                                                      300 30 100                                                                     400 60 98                                                                     101-14 100  3 98                                                                200 25 97                                                                      300 38 100                                                                     400 57 100                                                                    101-15 100  5 97                                                                200 25 97                                                                      300 40 100                                                                     400 40 99                                                                     101-16 100 10 97                                                                200 15 98                                                                      300 52 100                                                                     400  0 47                                                                     101-17 100  7 97                                                                200 25 94                                                                      300 40 98                                                                      400 33 97                                                                     101-18 100  7 96                                                                200 25 99                                                                      300 55 100                                                                     400 73 100                                                                  ______________________________________                                    

Percent inhibition data for the 400 g a.e./ha glyphosate rate in this test are unreliable and should be ignored. Neither oleth-20 (composition 101-05) nor steareth-20 (101-10) provided herbicidal effectiveness equal to Formulation J in this study, and no great or consistent further enhancement was obtained by adding butyl stearate.

Example 102

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 102a. Concentrate compositions 102-01 to 102-03 are oil-in-water emulsions and were prepared by process (vii). Compositions 102-04 to 102-18 all contain colloidal particulates and were prepared by process (ix). Different mixing methods were employed in the final stage of preparation of these compositions, as indicated in the column of Table 102a headed "Process".

The compositions of this example all showed acceptable storage stability. The compositions shown as containing colloidal particulate were not storage-stable unless the colloidal particulate was included as shown.

                                      TABLE 102a                                   __________________________________________________________________________                  % w/w                                                             Concentrate                                                                           Glyphosate                                                                           Butyl     Aerosil                                                                              Type of                                                                              Process                                       composition g a.e./l stearate Surfactant 380 surfactant (*)                  __________________________________________________________________________     102-01 163   0.5   5.0       oleth-20                                            102-02 163 0.5  5.0  steareth-20                                               102-03 163 0.5  5.0  ceteareth-27 A                                            102-04 360 1.0 10.0 1.25 ceteareth-15 A                                        102-05 360 1.0 10.0 1.25 ceteth-20 A                                           102-06 360 1.0 10.0 1.25 steareth-20 A                                         102-07 360 1.0 10.0 1.25 oleth-20 A                                            102-08 360 1.0 10.0 1.25 ceteareth-27 A                                        102-09 360 1.0 10.0 1.25 steareth-30 A                                         102-10 360  10.0 1.25 steareth-30 A                                            102-11 360 1.0 10.0 1.25 oleth-20 A                                            102-12 360 1.0 10.0 1.25 oleth-20 B                                            102-13 360 1.0 10.0 1.25 oleth-20 C                                            102-14 360 1.0 10.0 1.25 oleth-20 D                                            102-15 360 1.0 10.0 1.25 oleth-20 E                                            102-16 360 1.0 10.0 1.25 oleth-20 F                                            102-17 360 1.0 10.0 1.25 oleth-20 G                                            102-18 360 1.0 10.0 1.25 oleth-20 A                                          __________________________________________________________________________      (*) Process:                                                                   A Silverson mixer, medium screen, 3 minutes at 7000 rpm                        B Silverson mixer, coarse screen, 3 minutes at 7000 rpm                        C Fann mixer, 50% output, 5 minutes                                            D Turrax mixer, 3 minutes at 8000 rpm                                          E Overhead stirrer, low speed                                                  F Overhead stirrer, high speed                                                 G Hand shaking, 3 minutes                                                

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 19 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 102b.

                  TABLEe 102b                                                      ______________________________________                                                      Glyphosate rate                                                                           % Inhibition                                           Concentrate composition                                                                       g a.e./ha    ABUTH    ECHCF                                     ______________________________________                                         Formulation B  100          20       40                                           200 45 50                                                                      300 65 72                                                                      400 78 85                                                                     Formulation J 100 43 53                                                         200 80 80                                                                      300 96 82                                                                      400 99 94                                                                     102-01 100 45 57                                                                200 80 72                                                                      300 89 78                                                                      400 98 83                                                                     102-02 100 53 57                                                                200 80 78                                                                      300 89 77                                                                      400 93 83                                                                     102-03 100 45 60                                                                200 83 75                                                                      300 97 73                                                                      400 97 85                                                                     102-04 100 45 45                                                                200 80 80                                                                      300 83 83                                                                      400 95 95                                                                     102-05 100 42 42                                                                200 77 77                                                                      300 93 93                                                                      400 98 98                                                                     102-06 100 30 30                                                                200 42 42                                                                      300 27 30                                                                      400  3 20                                                                     102-07 100 40 40                                                                200 77 75                                                                      300 90 93                                                                      400 97 86                                                                     102-08 100 43 50                                                                200 80 80                                                                      300 92 93                                                                      400 96 98                                                                     102-09 100  0  2                                                                200 82 75                                                                      300 83 96                                                                      400 90 88                                                                     102-10 100 57 60                                                                200 80 70                                                                      300 88 88                                                                      400 95 93                                                                     102-11 100 35 47                                                                200 72 75                                                                      300 80 75                                                                      400 85 77                                                                     102-12 100 47 47                                                                200 72 77                                                                      300 80 90                                                                      400 86 78                                                                     102-13 100 55 50                                                                200 75 83                                                                      300 78 92                                                                      400 91 92                                                                     102-14 100 52 50                                                                200 75 78                                                                      300 83 88                                                                      400 99 92                                                                     102-15 100 47 47                                                                200 70 73                                                                      300 87 87                                                                      400 75 63                                                                     102-16 100 43 40                                                                200 78 75                                                                      300 88 88                                                                      400 87 91                                                                     102-17 100 43 43                                                                200 67 88                                                                      300 80 75                                                                      400 92 83                                                                     102-18 100 27 40                                                                200 63 57                                                                      300 82 73                                                                      400 87 70                                                                   ______________________________________                                    

Results obtained with composition 102-06 are out of line with other data in this Example and an error in formulation or application is suspected. Some differences in herbicidal effectiveness were evident when a composition containing 360 g a.e./l glyphosate, 1% butyl stearate, 10% oleth-20 and 1.25% Aerosil 380 was processed in different ways (102-11 to 102-17). However, as compositions 102-07 and 102-11 were identically processed yet differed in effectiveness, no firm conclusions can be drawn from this test.

Example 103

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 103a. Concentrate compositions 103-01 to 103-09 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 103-10 to 103-18 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix).

Compositions of this example containing 3% or 6% surfactant were not acceptably storage-stable except in the presence of colloidal particulate as shown.

                                      TABLE 103a                                   __________________________________________________________________________                 % w/w                                                              Composition                                                                          Glyphosate                                                                           Steareth-                                                                           Oleth-                                                                             Velvetex Type of                                            no. g a.e./l 20 20 AB-45 Aerosil Aerosil                                     __________________________________________________________________________     103-01                                                                               488   1.0               none                                               103-02 488 3.0    none                                                         103-03 488 6.0    none                                                         103-04 488  1.0   none                                                         103-05 488  3.0   none                                                         103-06 488  6.0   none                                                         103-07 488   1.0  none                                                         103-08 488   3.0  none                                                         103-09 488   4.6  none                                                         103-10 488 1.0   1.5 MOX-80/MOX-170 (1:1)                                      103-11 488 3.0   1.5 MOX-80/MOX-170 (1:1)                                      103-12 488 6.0   1.5 MOX-80/MOX-170 (1:1)                                      103-13 488  1.0  1.5 MOX-80/MOX-170 (1:1)                                      103-14 488  3.0  1.5 MOX-80/MOX-170 (1:1)                                      103-15 488  6.0  1.5 MOX-80/MOX-170 (1:1)                                      103-16 488   1.0 1.5 MOX-80/MOX-170 (1:1)                                      103-17 488   3.0 1.5 MOX-80/MOX-170 (1:1)                                      103-18 488   4.6 1.5 MOX-80/MOX-170 (1:1)                                    __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 103b.

                  TABLE 103b                                                       ______________________________________                                                      Glyphosate rate                                                                           % Inhibition                                           Concentrate composition                                                                       g a.e./ha    ABUTH    ECHCF                                     ______________________________________                                         Formulation B  100          10       40                                           200 38 67                                                                      300 70 80                                                                      400 86 92                                                                     Formulation J 100 43 58                                                         200 65 82                                                                      300 91 94                                                                      400 100   95                                                                  103-01 100 23 60                                                                200 40 65                                                                      300 73 87                                                                      400 80 92                                                                     103-02 100 38 67                                                                200 77 82                                                                      300 95 83                                                                      400 99 93                                                                     103-03 100 33 67                                                                200 78 73                                                                      300 90 94                                                                      400 100  96                                                                   103-04 100 23 63                                                                200 48 81                                                                      300 68 87                                                                      400 72 88                                                                     103-05 100 30 63                                                                200 63 80                                                                      300 78 89                                                                      400 95 93                                                                     103-06 100 25 85                                                                200 68 93                                                                      300 77 93                                                                      400 99 95                                                                     103-07 100 13 60                                                                200 42 80                                                                      300 57 95                                                                      400 92 96                                                                     103-08 100 20 73                                                                200 43 92                                                                      300 83 93                                                                      400 72 96                                                                     103-09 100 30 73                                                                200 50 94                                                                      300 65 96                                                                      400 75 98                                                                     103-10 100 10 65                                                                200 53 88                                                                      300 72 94                                                                      400 83 95                                                                     103-11 100 15 50                                                                200 57 77                                                                      300 82 95                                                                      400 92 97                                                                     103-12 100 30 70                                                                200 68 98                                                                      300 78 97                                                                      400 96 98                                                                     103-13 100 15 77                                                                200 43 93                                                                      300 68 95                                                                      400 77 99                                                                     103-14 100 10 73                                                                200 40 93                                                                      300 68 98                                                                      400 78 98                                                                     103-15 100 missing missing                                                      200 missing missing                                                            300 missing missing                                                            400 missing missing                                                           103-16 100  0 60                                                                200 30 93                                                                      300 40 99                                                                      400 50 99                                                                     103-17 100  2 83                                                                200 43 99                                                                      300 67 100                                                                     400 67 100                                                                    103-18 100  5 95                                                                200 37 100                                                                     300 60 100                                                                     400 78 100                                                                  ______________________________________                                    

In high-load (488 g a.e./l) glyphosate compositions, steareth-20 at 3% or 6% provided greater herbicidal effectiveness in this test than the same concentrations of oleth-20. Even at just 3%, steareth-20 (composition 103-02) gave effectiveness equal to commercial standard Formulation J. Addition of a blend of colloidal particulates to stabilize the composition (103-11) slightly reduced effectiveness in this study.

Example 104

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 104a. Concentrate compositions 104-01 to 104-04 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 104-08 to 104-18 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix). Concentrate compositions 104-05 to 104-07 contain colloidal particulate but no surfactant.

All compositions of this example except 104-01 to 104-03 were acceptably storage-stable.

                                      TABLE 104a                                   __________________________________________________________________________                 % w/w                                                              Concentrate                                                                          Glyphosate                                                                           Steareth-                                                                           Steareth-                                                                           MON    Type of                                             composition g a.e./l 20 100 0818 Aerosil Aerosil                             __________________________________________________________________________     104-01                                                                               488   3.0                                                                  104-02 488 4.5                                                                 104-03 488 6.0                                                                 104-04 488   3.0                                                               104-05 488    1.5 380                                                          104-06 488    1.5 MOX-80/MOX-170 (1:1)                                         104-07 488    3.0 MOX-80/380(1:1)                                              104-08 488  1.5                                                                104-09 488 3.0  3.0 1.5 380                                                    104-10 488 4.5  3.0 1.5 380                                                    104-11 488 6.0  3.0 1.5 380                                                    104-12 488 3.0  3.0 1.5 MOX-80/MOX-170 (1:1)                                   104-13 488 4.5  3.0 1.5 MOX-80/MOX-170 (1:1)                                   104-14 488 6.0  3.0 1.5 MOX-80/MOX-170 (1:1)                                   104-15 488 3.0  3.0 1.5 MOX-80/380 (1:1)                                       104-16 488 4.5  3.0 1.5 MOX-80/380 (1:1)                                       104-17 488 6.0  3.0 1.5 MOX-80/380 (1:1)                                       104-18 488  4.5 3.0 1.5 MOX-80/MOX-170 (1:1)                                 __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 21 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 104b.

                  TABLE 104b                                                       ______________________________________                                                      Glyphosate rate                                                                           % Inhibition                                           Concentrate composition                                                                       g a.e./ha    ABUTH    ECHCF                                     ______________________________________                                         Formulation B  100           2       23                                           200 18 50                                                                      300 42 67                                                                      400 63 80                                                                     Formulation J 100 20 47                                                         200 40 86                                                                      300 83 98                                                                      400 93 98                                                                     104-01 100 10 75                                                                200 62 83                                                                      300 80 96                                                                      400 93 99                                                                     104-02 100 40 60                                                                200 77 92                                                                      300 87 97                                                                      400 93 99                                                                     104-03 100 23 40                                                                200 38 63                                                                      300 78 91                                                                      400 97 91                                                                     104-04 100 20 38                                                                200 23 77                                                                      300 43 94                                                                      400 73 94                                                                     104-05 100  7 30                                                                200 25 37                                                                      300 42 60                                                                      400 67 63                                                                     104-06 100  7 30                                                                200 20 53                                                                      300 52 67                                                                      400 83 67                                                                     104-07 100  5 35                                                                200 20 63                                                                      300 57 80                                                                      400 43 85                                                                     104-08 100 22 83                                                                200 47 99                                                                      300 86 98                                                                      400 78 100                                                                    104-09 100 12 45                                                                200 25 77                                                                      300 40 83                                                                      400 37 95                                                                     104-10 100 13 53                                                                200 73 99                                                                      300 85 98                                                                      400 99 99                                                                     104-11 100 25 50                                                                200 60 88                                                                      300 93 99                                                                      400 99 99                                                                     104-12 100 25 45                                                                200 57 88                                                                      300 85 97                                                                      400 100  94                                                                   104-13 100 30 52                                                                200 68 87                                                                      300 93 99                                                                      400 100  92                                                                   104-14 100 40 45                                                                200 73 88                                                                      300 81 98                                                                      400 100  99                                                                   104-15 100  8 57                                                                200 33 96                                                                      300 81 99                                                                      400 95 99                                                                     104-16 100 10 62                                                                200 48 83                                                                      300 99 98                                                                      400 100  100                                                                  104-17 100 27 58                                                                200 65 92                                                                      300 75 98                                                                      400 93 99                                                                     104-18 100  5 40                                                                200 33 87                                                                      300 55 98                                                                      400 75 98                                                                   ______________________________________                                    

Among stabilized high-load (488 g a.e./l) glyphosate compositions providing herbicidal effectiveness superior to commercial standard Formulation J, at least on ABUTH, were 104-10 and 104-11 (respectively 4.5% and 6% steareth-20+3% MON 0818+1.5% Aerosil 380), 104-13 (4.5% steareth-20+3% MON 0818+1.5% MOX-80/MOX-170 blend) and 104-16 (4.5% steareth-20+3% MON 0818+1.5% Aerosil MOX-80/380 blend). The relatively poor performance of composition 104-04 and the good performance of composition 104-02 shows that the excellent results obtained with the stabilized compositions listed above are primarily attributable to the steareth-20 component.

Example 105

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 105a. Concentrate compositions 105-01 to 105-09 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 105-10 to 105-18 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix).

Compositions of this example containing 3% or 6% surfactant were not acceptably storage-stable except in the presence of colloidal particulate as shown.

                                      TABLE 105a                                   __________________________________________________________________________                 % w/w                                                              Concentrate                                                                          Glyphosate                                                                           Steareth-                                                                           Oleth-                                                                              Velvetex Type of                                           composition g a.e./l 20 20 AB-45 Aerosil Aerosil                             __________________________________________________________________________     105-01                                                                               488   1.5                none                                              105-02 488 3.0    none                                                         105-03 488 6.0    none                                                         105-04 488  1.5   none                                                         105-05 488  3.0   none                                                         105-06 488  6.0   none                                                         105-07 488   1.5  none                                                         105-08 488   3.0  none                                                         105-09 488   4.5  none                                                         105-10 488 1.5   1.5 MOX-80/380 (1:1)                                          105-11 488 3.0   1.5 MOX-80/380 (1:1)                                          105-12 488 6.0   1.5 MOX-80/380 (1:1)                                          105-13 488  1.5  1.5 MOX-80/380 (1:1)                                          105-14 488  3.0  1.5 MOX-80/380 (1:1)                                          105-15 488  6.0  1.5 MOX-80/380 (1:1)                                          105-16 488   1.5 1.5 MOX-80/380 (1:1)                                          105-17 488   3.0 1.5 MOX-80/380 (1:1)                                          105-18 488   4.5 1.5 MOX-80/380 (1:1)                                        __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 15 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 22 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 105b.

                  TABLE 105b                                                       ______________________________________                                                    Glyphosate                                                            Concentrate rate % Inhibition                                                composition                                                                               g a.e./ha     ABUTH    ECHCF                                        ______________________________________                                         Formulation B                                                                             100            0       10                                              200  3 27                                                                      300 13 30                                                                      400 33 40                                                                     Formulation J 100  2 53                                                         200 30 97                                                                      300 70 99                                                                      400 80 99                                                                     105-01 100  5 67                                                                200 30 89                                                                      300 58 98                                                                      400 80 100                                                                    105-02 100 20 60                                                                200 45 90                                                                      300 78 99                                                                      400 80 100                                                                    105-03 100 20 57                                                                200 47 93                                                                      300 78 96                                                                      400 83 98                                                                     105-04 100  3 57                                                                200 30 83                                                                      300 63 99                                                                      400 82 98                                                                     105-05 100  5 53                                                                200 27 83                                                                      300 47 98                                                                      400 77 100                                                                    105-06 100  5 40                                                                200 23 70                                                                      300 47 92                                                                      400 77 99                                                                     105-07 100  3 53                                                                200 30 85                                                                      300 60 94                                                                      400 72 97                                                                     105-08 100  3 50                                                                200 22 88                                                                      300 53 97                                                                      400 80 100                                                                    105-09 100  0 40                                                                200 20 83                                                                      300 40 99                                                                      400 67 99                                                                     105-10 100  0 40                                                                200 27 60                                                                      300 47 83                                                                      400 78 94                                                                     105-11 100  5 47                                                                200 25 77                                                                      300 57 96                                                                      400 87 97                                                                     105-12 100 15 43                                                                200 52 88                                                                      300 87 98                                                                      400 87 98                                                                     105-13 100  0 40                                                                200 17 70                                                                      300 35 83                                                                      400 53 88                                                                     105-14 100  0 33                                                                200 18 67                                                                      300 28 90                                                                      400 62 98                                                                     105-15 100  2 33                                                                200 25 70                                                                      300 53 85                                                                      400 72 97                                                                     105-16 100  0 30                                                                200 17 50                                                                      300 27 67                                                                      400 72 87                                                                     105-17 100  0  0                                                                200  7 63                                                                      300 32 88                                                                      400 47 90                                                                     105-18 100  0  5                                                                200 12 60                                                                      300 25 83                                                                      400 45 97                                                                   ______________________________________                                    

Compositions containing steareth-20 generally performed better than counterparts containing oleth-20 in this study, both in the presence and in the absence of colloidal particulates.

Example 106

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 106a. All contain colloidal particulates and were prepared by process (ix).

The compositions of this example all showed acceptable storage stability. The compositions shown as containing colloidal particulate were not storage-stable unless the colloidal particulate was included as shown.

                                      TABLE 106a                                   __________________________________________________________________________     % w/w                                                                          Concentrate                                                                          Glyphosate    Aerosil                                                                            Type of                                                                               Type of                                           composition a.e. Oil Surfactant 380 oil surfactant                           __________________________________________________________________________     106-01                                                                               31    1.0                                                                               10.0 1.25                                                                               Butyl stearate                                                                        steareth-20                                       106-02 31 1.0 10.0 1.25 Butyl stearate oleth-20                                106-03 31 1.0 10.0 1.25 Butyl stearate steareth-30                             106-04 31  10.0 1.25 none steareth-30                                        __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Treatments were applied at four different hours of the day. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 22 days after application.

Formulation J was applied as a comparative treatment. Results, averaged for all replicates of each treatment, are shown in Table 106b.

                  TABLE 106b                                                       ______________________________________                                                   Hour    Glyphosate                                                     Concentrate when rate % Inhibition                                           composition                                                                              applied g a.e./ha   ABUTH  ECHCF                                     ______________________________________                                         Formulation J                                                                            1000    100          5     33                                            200 42 75                                                                      300 67 83                                                                      400 77 93                                                                    106-01 1000 100  7 33                                                            200 40 70                                                                      300 50 82                                                                      400 78 91                                                                    106-02 1000 100 18 33                                                            200 37 73                                                                      300 48 91                                                                      400 80 92                                                                    106-03 1000 100 30 33                                                            200 40 75                                                                      300 82 85                                                                      400 83 80                                                                    106-04 1000 100 30 30                                                            200 43 78                                                                      300 78 92                                                                      400 93 95                                                                    Formulation J 1200 100  5 38                                                     200 35 87                                                                      300 53 96                                                                      400 88 99                                                                    106-01 1200 100 10 30                                                            200 47 91                                                                      300 70 89                                                                      400 78 97                                                                    106-02 1200 100  5 37                                                            200 40 75                                                                      300 48 87                                                                      400 70 94                                                                    106-03 1200 100 20 37                                                            200 50 82                                                                      300 78 98                                                                      400 83 97                                                                    106-04 1200 100 33 33                                                            200 45 93                                                                      300 75 98                                                                      400 95 100                                                                   Formulation J 1400 100 15 40                                                     200 30 90                                                                      300 55 100                                                                     400 80 100                                                                   106-01 1400 100 17 40                                                            200 45 70                                                                      300 75 97                                                                      400 80 98                                                                    106-02 1400 100 17 47                                                            200 35 83                                                                      300 67 97                                                                      400 63 97                                                                    106-03 1400 100 30 40                                                            200 63 80                                                                      300 77 97                                                                      400 78 100                                                                   106-04 1400 100 23 40                                                            200 45 87                                                                      300 73 100                                                                     400 78 100                                                                   Formulation J 1600 100 10 37                                                     200 32 83                                                                      300 52 97                                                                      400 75 98                                                                    106-01 1600 100 27 43                                                            200 40 89                                                                      300 77 99                                                                      400 95 99                                                                    106-02 1600 100 20 53                                                            200 40 95                                                                      300 53 98                                                                      400 80 98                                                                    106-03 1600 100 27 60                                                            200 60 93                                                                      300 78 97                                                                      400 96 100                                                                   106-04 1600 100 15 37                                                            200 43 83                                                                      300 67 97                                                                      400 78 96                                                                  ______________________________________                                    

Composition 106-03 illustrates the consistency of high-level performance obtainable with, in this case, steareth-30 at an approximately 1:3 weight/weight ratio to glyphosate a.e., together with a small amount of butyl stearate and Aerosil 380. An average of percent inhibition of ABUTH across all four glyphosate rates shows the following comparison of 106-03 with Formulation J, applied at four different hours of the day:

    ______________________________________                                         Hour       Formulation J                                                                             Composition 106-03                                       ______________________________________                                         1000       48         59                                                         1200 45 58                                                                     1400 48 62                                                                     1600 42 65                                                                   ______________________________________                                    

Example 107

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 107a. Concentrate compositions 107-01 to 107-07 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 107-08 to 107-18 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix).

Compositions 107-01 to 107-06 were not acceptably storage-stable. All other compositions showed acceptable storage stability.

                  TABLE 107a                                                       ______________________________________                                         Glypho-      % w/w                                                             Concentrate                                                                            sate     Steareth-                                                                               Steareth-                                                                             Agrimul                                                                               Aerosil                                  composition g a.e./l 30 20 PG-2069 380                                       ______________________________________                                         107-01  488      3.00                                                            107-02 488 4.50                                                                107-03 488 6.00                                                                107-04 488  3.00                                                               107-05 488  4.50                                                               107-06 488  6.00                                                               107-07 488   2.0                                                               107-08 488 3.00                                                                107-09 488 4.50   1.5                                                          107-10 488 6.00   1.5                                                          107-11 488  3.00  1.5                                                          107-12 488  4.50  1.5                                                          107-13 488  6.00  1.5                                                          107-14 488 1.50 1.50  1.5                                                      107-15 488 2.25 2.25  1.5                                                      107-16 488 3.00 3.00  1.5                                                      107-17 488 2.25 2.25 2.0 1.5                                                   107-18 488 3.00 3.00 2.0 1.5                                                 ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 23 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 107b.

                  TABLE 107b                                                       ______________________________________                                                    Glyphosate                                                            Concentrate rate % Inhibition                                                composition                                                                               g a.e./ha     ABUTH    ECHCF                                        ______________________________________                                         Formulation B                                                                             100            2       20                                              200 22 33                                                                      300 35 67                                                                      400 68 73                                                                     Formulation J 100 32 63                                                         200 78 90                                                                      300 83 93                                                                      400 92 97                                                                     107-01 100 38 57                                                                200 50 63                                                                      300 62 80                                                                      400 75 89                                                                     107-02 100 20 57                                                                200 63 70                                                                      300 75 88                                                                      400 80 96                                                                     107-03 100 47 53                                                                200 72 80                                                                      300 87 96                                                                      400 100  99                                                                   107-04 100 33 30                                                                200 48 60                                                                      300 75 73                                                                      400 90 83                                                                     107-05 100 10 30                                                                200 43 50                                                                      300 68 82                                                                      400 83 92                                                                     107-06 100 22 40                                                                200 43 50                                                                      300 75 83                                                                      400 83 87                                                                     107-07 100 10 37                                                                200 40 63                                                                      300 78 86                                                                      400 95 96                                                                     107-08 100 23 43                                                                200 68 63                                                                      300 92 88                                                                      400 98 93                                                                     107-09 100 47 57                                                                200 78 70                                                                      300 95 92                                                                      400 100  96                                                                   107-10 100 37 57                                                                200 85 68                                                                      300 92 85                                                                      400 100  93                                                                   107-11 100 28 43                                                                200 63 73                                                                      300 85 83                                                                      400 95 96                                                                     107-12 100 40 53                                                                200 75 88                                                                      300 90 92                                                                      400 100  97                                                                   107-13 100 40 53                                                                200 75 75                                                                      300 99 92                                                                      400 100  98                                                                   107-14 100 30 43                                                                200 68 72                                                                      300 83 82                                                                      400 96 97                                                                     107-15 100 38 47                                                                200 77 72                                                                      300 94 92                                                                      400 100  96                                                                   107-16 100 33 43                                                                200 75 67                                                                      300 92 88                                                                      400 100  94                                                                   107-17 100 25 43                                                                200 68 82                                                                      300 78 96                                                                      400 99 96                                                                     107-18 100 13 37                                                                200 72 70                                                                      300 87 80                                                                      400 99 85                                                                   ______________________________________                                    

Several stabilized high-load (488 g a.e./l) glyphosate compositions of this Example provided herbicidal effectiveness equal or superior, at least on ABUTH, to that obtained with commercial standard Formulation J.

Example 108

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 108a. Concentrate compositions 108-12 to 108-14 are aqueous solution concentrates and were prepared by process (viii). Concentrate compositions 108-01 to 108-11 and 108-15 to 108-17 are aqueous solution concentrates containing colloidal particulates and were prepared by process (ix).

                                      TABLE 108a                                   __________________________________________________________________________                 % w/w                                                              Conc. Glyphosate                                                                           Steareth-                                                                           Ethomeen                                                                            Propylene                                                                               Type of                                           comp. g a.e./l 20 T/25 glycol Aerosil Aerosil                                __________________________________________________________________________     108-01                                                                               488   3.0            0.8 380                                               108-02 488 6.0   1.5 MOX-80/MOX-170 (1:1)                                      108-03 488 4.5   1.5 380                                                       108-04 488 4.5 2.25 0.5 1.5 MOX-80/380 (1:2)                                   108-05 488 4.5  0.5 1.5 MOX-80/380 (1:2)                                       108-06 488 6.0  0.5 1.5 MOX-80/380 (1:2)                                       108-07 488 3.0 1.50 0.5 1.5 MOX-80/380 (1:2)                                   108-08 488 6.0 3.00 0.5 1.5 MOX-80/380 (1:2)                                   108-09 488 3.0 1.50 0.5 1.5 380                                                108-10 488 4.5 2.25 0.5 1.5 380                                                108-11 488 6.0 3.00 0.5 1.5 380                                                108-12 488  1.50 0.5  none                                                     108-13 488  2.25 0.5  none                                                     108-14 488  3.00 0.5  none                                                     108-15 488  1.50 0.5 1.5 MOX-80/380 (1:2)                                      108-16 488  2.25 0.5 1.5 MOX-80/380 (1:2)                                      108-17 488  3.00 0.5 1.5 MOX-80/380 (1:2)                                    __________________________________________________________________________

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 20 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 108b.

                  TABLE 108b                                                       ______________________________________                                                    Glyphosate                                                            Concentrate rate % Inhibition                                                composition                                                                               g a.e./ha     ABUTH    ECHCF                                        ______________________________________                                         Formulation B                                                                             100            0        3                                              200 10 12                                                                      300 43 22                                                                      400 47 27                                                                     Formulation J 100 13 15                                                         200 25 22                                                                      300 58 53                                                                      400 68 82                                                                     108-01 100 30 20                                                                200 60 53                                                                      300 73 88                                                                      400 87 96                                                                     108-02 100 40 23                                                                200 63 55                                                                      300 88 87                                                                      400 93 93                                                                     108-03 100 42 20                                                                200 72 55                                                                      300 82 83                                                                      400 90 88                                                                     108-04 100 60 32                                                                200 70 57                                                                      300 90 88                                                                      400 90 93                                                                     108-05 100 47 32                                                                200 67 57                                                                      300 88 85                                                                      400 94 88                                                                     108-06 100 33 37                                                                200 68 67                                                                      300 82 80                                                                      400 90 88                                                                     108-07 100 35 37                                                                200 67 70                                                                      300 87 85                                                                      400 97 93                                                                     108-08 100 32 35                                                                200 67 77                                                                      300 85 92                                                                      400 97 95                                                                     108-09 100 27 33                                                                200 57 67                                                                      300 88 83                                                                      400 93 95                                                                     108-10 100 13 33                                                                200 62 58                                                                      300 80 80                                                                      400 92 92                                                                     108-11 100 13 20                                                                200 60 57                                                                      300 88 63                                                                      400 93 82                                                                     108-12 100 10 27                                                                200 53 53                                                                      300 70 67                                                                      400 88 85                                                                     108-13 100  3 28                                                                200 50 57                                                                      300 67 70                                                                      400 90 82                                                                     108-14 100  3 28                                                                200 55 57                                                                      300 70 83                                                                      400 87 87                                                                     108-15 100 10 20                                                                200 58 43                                                                      300 70 72                                                                      400 83 85                                                                     108-16 100 12 22                                                                200 55 57                                                                      300 73 77                                                                      400 92 90                                                                     108-17 100  7 20                                                                200 53 55                                                                      300 70 75                                                                      400 85 88                                                                   ______________________________________                                    

Several stabilized high-load (488 g a.e./l) glyphosate compositions of this Example provided herbicidal effectiveness equal or superior, on both ABUTH and ECHCF, to that obtained with commercial standard Formulation J.

Example 109

Glyphosate-containing spray compositions were prepared by tank-mixing Formulation B with excipients as shown in Table 109.

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 22 days after application. Results, averaged for all replicates of each treatment, are shown in Table 109.

                  TABLE 109                                                        ______________________________________                                                  Glypho-                                                                  sate  Ratio                                                                   Glyphosate rate  add./ % Inhibition                                          composition                                                                             g a.e./ha                                                                               Additive  a.e. ABUTH  ECHCF                                  ______________________________________                                         Formulation B                                                                           150      none           18     25                                        250   73 58                                                                    350   80 82                                                                   Formulation J 150 none  47 90                                                   250   77 93                                                                    350   95 94                                                                   Formulation B 150 steareth-10 1:0.3 53 88                                       250   83 94                                                                    350   98 98                                                                   Formulation B 150 steareth-10 1:1   48 73                                       250   67 97                                                                    350   93 99                                                                   Formulation B 150 steareth-10 1:1.5 52 60                                       250   65 95                                                                    350   86 99                                                                   Formulation B 150 steareth-10 1:3   48 73                                       250   65 83                                                                    350   80 98                                                                   Formulation B 150 steareth-10 1:6   50 81                                       250   60 87                                                                    350   85 97                                                                   Formulation B 150 steareth-20 1:0.3 76 92                                       250   100  93                                                                  350   100  99                                                                 Formulation B 150 steareth-20 1:1   65 75                                       250   94 96                                                                    350   99 99                                                                   Formulation B 150 steareth-20 1:1.5 52 95                                       250   84 92                                                                    350   98 98                                                                   Formulation B 150 steareth-20 1:3   53 82                                       250   82 100                                                                   350   98 93                                                                   Formulation B 150 steareth-20 1:6   47 62                                       250   68 93                                                                    350   92 97                                                                   Formulation B 150 steareth-30 1:0.3 63 88                                       250   97 100                                                                   350   100  100                                                                Formulation B 150 steareth-30 1:1   53 72                                       250   88 96                                                                    350   97 97                                                                   Formulation B 150 steareth-30 1:1.5 50 79                                       250   81 89                                                                    350   96 100                                                                  Formulation B 150 steareth-30 1:3   50 67                                       250   78 88                                                                    350   97 91                                                                   Formulation B 150 steareth-30 1:6   47 58                                       250   75 99                                                                    350   89 99                                                                   Formulation B 150 ceteareth-30 1:0.3 55 86                                      250   89 91                                                                    350   99 100                                                                  Formulation B 150 ceteareth-30 1:1   50 86                                      250   85 95                                                                    350   97 100                                                                  Formulation B 150 ceteareth-30 1:1.5 43 75                                      250   80 100                                                                   350   88 98                                                                   Formulation B 150 ceteareth-30 1:3   33 73                                      250   60 92                                                                    350   94 100                                                                  Formulation B 150 ceteareth-30 1:6   37 73                                      250   53 89                                                                    350   88 100                                                                  Formulation B 150 Ethomeen 1:0.3 67 90                                          250 T/25  92 99                                                                350   100  100                                                                Formulation B 150 Ethomeen 1:1   58 94                                          250 T/25  83 96                                                                350   93 98                                                                   Formulation B 150 Ethomeen 1:1.5 50 73                                          250 T/25  86 100                                                               350   99 100                                                                  Formulation B 150 Ethomeen 1:3   45 83                                          250 T/25  89 95                                                                350   100  100                                                                Formulation B 150 Ethomeen 1:6   35 82                                          250 T/25  73 98                                                                350   88 98                                                                 ______________________________________                                    

Steareth-20, steareth-30 and ceteareth-30 were more effective additives for Formulation B than steareth-10 in this study.

Example 110

Aqueous spray compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 110a. Process (iii) was followed for spray compositions 110-01 to 110-22 and 110-26 to 110-72, using soybean lecithin (45% phospholipid, Avanti). Process (i) was followed for spray compositions 110-23 to 110-25.

                  TABLE 110a                                                       ______________________________________                                                 % w/w                                                                  Spray                   Butyl   MON                                              compositions Lecithin stearate 0818                                          ______________________________________                                         110-01    0.10          0.10                                                     110-02 0.10 0.08                                                               110-03 0.10 0.05                                                               110-04 0.10 0.03                                                               110-05 0.10 0.01                                                               110-06 0.08 0.10                                                               110-07 0.05 0.10                                                               110-08 0.03 0.10                                                               110-09 0.01 0.10                                                               110-10 0.08 0.01                                                               110-11 0.05 0.01                                                               110-12 0.03 0.01                                                               110-13 0.01 0.01                                                               110-14 0.01 0.03                                                               110-15 0.01 0.05                                                               110-16 0.01 0.08                                                               110-17 0.03 0.03                                                               110-18 0.05 0.05                                                               110-19 0.08 0.08                                                               110-20 0.08 0.03                                                               110-21 0.03 0.08                                                               110-22 0.05                                                                    110-23  0.05                                                                   110-24   0.09                                                                  110-25   0.03                                                                  110-26 0.09 0.02 0.09                                                          110-27 0.09 0.02 0.05                                                          110-28 0.01 0.01 0.01                                                          110-29 0.01 0.01 0.03                                                          110-30 0.01 0.01 0.05                                                          110-31 0.01 0.01 0.08                                                          110-32 0.01 0.01 0.10                                                          110-33 0.01 0.05 0.01                                                          110-34 0.01 0.05 0.03                                                          110-35 0.01 0.05 0.05                                                          110-36 0.01 0.05 0.08                                                          110-37 0.01 0.05 0.10                                                          110-38 0.01 0.10 0.01                                                          110-39 0.01 0.10 0.03                                                          110-40 0.01 0.10 0.05                                                          110-41 0.01 0.10 0.08                                                          110-42 0.01 0.10 0.10                                                          110-43 0.05 0.01 0.01                                                          110-44 0.05 0.01 0.03                                                          110-45 0.05 0.01 0.05                                                          110-46 0.05 0.01 0.08                                                          110-47 0.05 0.01 0.10                                                          110-48 0.05 0.05 0.01                                                          110-49 0.05 0.05 0.03                                                          110-50 0.05 0.05 0.05                                                          110-51 0.05 0.05 0.08                                                          110-52 0.05 0.05 0.10                                                          110-53 0.05 0.10 0.01                                                          110-54 0.05 0.10 0.03                                                          110-55 0.05 0.10 0.05                                                          110-56 0.05 0.10 0.08                                                          110-57 0.05 0.10 0.10                                                          110-58 0.10 0.01 0.01                                                          110-59 0.10 0.01 0.03                                                          110-60 0.10 0.01 0.05                                                          110-61 0.10 0.01 0.08                                                          110-62 0.10 0.01 0.10                                                          110-63 0.10 0.05 0.01                                                          110-64 0.10 0.05 0.03                                                          110-65 0.10 0.05 0.05                                                          110-66 0.10 0.05 0.08                                                          110-67 0.10 0.05 0.10                                                          110-68 0.10 0.10 0.01                                                          110-69 0.10 0.10 0.03                                                          110-70 0.10 0.10 0.05                                                          110-71 0.10 0.10 0.08                                                          110-72 0.10 0.10 0.10                                                        ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 110b.

                  TABLE 110b                                                       ______________________________________                                                     Glyphosate                                                           Spray rate % Inhibition                                                      compositions                                                                               g a.e./ha   ABUTH    ECHCF                                         ______________________________________                                         Formulation C                                                                              280         71       73                                              Formulation J 280 65 77                                                        110-01 280 60 49                                                               110-02 280 46 47                                                               110-03 280 34 48                                                               110-04 280 33 35                                                               110-05 280 50 33                                                               110-06 280 49 52                                                               110-07 280 39 42                                                               110-08 280 48 38                                                               110-09 280 51 42                                                               110-10 280 37 30                                                               110-11 280 48 30                                                               110-12 280 56 34                                                               110-13 280 41 45                                                               110-14 280 52 56                                                               110-15 280 38 40                                                               110-16 280 53 33                                                               110-17 280 45 40                                                               110-18 280 52 38                                                               110-19 280 37 34                                                               110-20 280 36 28                                                               110-21 280 40 38                                                               110-22 280 44 47                                                               110-23 280 60 42                                                               110-24 280 92 76                                                               110-25 280 87 69                                                               110-26 280 89 88                                                               110-27 280 79 80                                                               110-28 280 74 73                                                               110-29 280 91 76                                                               110-30 280 94 92                                                               110-31 280 87 81                                                               110-32 280 93 77                                                               110-33 280 88 73                                                               110-34 280 92 85                                                               110-35 280 90 82                                                               110-36 280 92 77                                                               110-37 280 87 77                                                               110-38 280 88 77                                                               110-39 280 84 74                                                               110-40 280 87 68                                                               110-41 280 93 76                                                               110-42 280 94 78                                                               110-43 280 80 59                                                               110-44 280 69 54                                                               110-45 280 88 74                                                               110-46 280 94 79                                                               110-47 280 95 79                                                               110-48 280 71 63                                                               110-49 280 81 72                                                               110-50 280 81 79                                                               110-51 280 79 85                                                               110-52 280 98 69                                                               110-53 280 69 70                                                               110-54 280 74 69                                                               110-55 280 84 78                                                               110-56 280 86 68                                                               110-57 280 98 82                                                               110-58 280 71 69                                                               110-59 280 95 79                                                               110-60 280 92 70                                                               110-61 280 93 70                                                               110-62 280 98 80                                                               110-63 280 81 74                                                               110-64 280 84 73                                                               110-65 280 89 70                                                               110-66 280 91 65                                                               110-67 280 94 81                                                               110-68 280 87 81                                                               110-69 280 72 79                                                               110-70 280 87 76                                                               110-71 280 94 71                                                               110-72 280 97 73                                                             ______________________________________                                    

Compositions outperforming commercial standard Formulations C and J on both ABUTH and ECHCF in this test included 110-26, 110-27, 110-30, 110-34, 110-35, 110-51 and 110-57, all containing lecithin, butyl stearate and MON 0818.

Example 111

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 111a. Concentrate compositions 111-01 to 111-06 were prepared by process (x), using soybean lecithin (45% phospholipid, Avanti). Compositions 111-07 was prepared by precess (viii).

                  TABLE 111a                                                       ______________________________________                                                        % w/w                                                           Concentrate                                                                               Glyphosate         Butyl Ethomeen                                     composition g a.e./l Lecithin stearate T/25                                  ______________________________________                                         111-01     200       6.0      2     6.0                                          111-02 200  3 6.0                                                              111-03 200  1.5 9.0                                                            111-04 200  3 9.0                                                              111-05 200 6.0 1.5 9.0                                                         111-06 200 6.0 1.5 3.0                                                         111-07 200   9.0                                                             ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 16 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 15 days after application.

Formulations C and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 111b.

                  TABLE 111b                                                       ______________________________________                                                    Glyphosate                                                            Concentrate rate % Inhibition                                                composition                                                                               g a.e./ha     ABUTH    ECHCF                                        ______________________________________                                         Formulation B                                                                             150           29       22                                              250 41 29                                                                      350 53 32                                                                      450 68 35                                                                     Formulation J 150 43 32                                                         250 76 43                                                                      350 86 47                                                                      450 94 66                                                                     111-01 150 67 33                                                                250 85 40                                                                      350 96 71                                                                      450 97 59                                                                     111-02 150 65 36                                                                250 81 52                                                                      350 97 68                                                                      450 98 62                                                                     111-03 150 67 40                                                                250 85 77                                                                      350 94 77                                                                      450 97 63                                                                     111-04 150 69 38                                                                250 86 58                                                                      350 93 84                                                                      450 98 62                                                                     111-05 150 73 40                                                                250 83 53                                                                      350 93 75                                                                      450 96 61                                                                     111-06 150 45 30                                                                250 71 38                                                                      350 91 45                                                                      450 89 39                                                                     111-07 150 59 39                                                                250 83 44                                                                      350 95 63                                                                      450 95 70                                                                   ______________________________________                                    

Data for the 450 g a.e./ha glyphosate rate in this study are unreliable. Application error is suspected. The high levels of Ethomeen T/25 included in compositions of this Example tends to obscure the effects of lecithin and butyl stearate, but composition 111-05, for example, showed outstanding effectiveness.

Example 112

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 112a. Process (vii) was followed for concentrate composition 112-08 and process (x) for concentrate compositions 112-01 to 112-07 and 112-09, using soybean lecithin (45% phospholipid, Avanti).

                  TABLE 112a                                                       ______________________________________                                                      % w/w                                                             Concentrate                                                                             Glyphosate          Butyl                                               composition g a.e./l Lecithin stearate MON 0818                              ______________________________________                                         112-01   220       4.0             6.0                                           112-02 220 4.0 0.5 6.0                                                         112-03 220 4.0 1.0 6.0                                                         112-04 220 4.0 2.0 6.0                                                         112-05 220 2.0 0.5 2.0                                                         112-06 220 2.0 0.5 4.0                                                         112-07 220 2.0 0.5 6.0                                                         112-08 220  0.5 6.0                                                            112-09 220 6.0 1.5 6.0                                                       ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 17 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and C were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 112b.

                  TABLE 112b                                                       ______________________________________                                                    Glyphosate                                                            Concentrate rate % Inhibition                                                composition                                                                               g a.e./ha     ABUTH    ECHCF                                        ______________________________________                                         Formulation B                                                                             150           40       59                                              250 68 61                                                                      350 90 91                                                                      450 93 94                                                                     Formulation C 150 74 78                                                         250 93 90                                                                      350 97 96                                                                      450 100  94                                                                   112-01 150 79 85                                                                250 93 98                                                                      350 96 97                                                                      450 97 95                                                                     112-02 150 71 87                                                                250 93 96                                                                      350 96 94                                                                      450 98 94                                                                     112-03 150 87 99                                                                250 94 100                                                                     350 99 97                                                                      450 97 94                                                                     112-04 150 89 100                                                               250 94 99                                                                      350 97 98                                                                      450 98 95                                                                     112-05 150 73 100                                                               250 90 100                                                                     350 95 98                                                                      450 96 94                                                                     112-06 150 80 99                                                                250 94 96                                                                      350 95 100                                                                     450 99 98                                                                     112-07 150 88 83                                                                250 94 92                                                                      350 96 92                                                                      450 100  90                                                                   112-08 150 81 91                                                                250 92 96                                                                      350 97 89                                                                      450 99 92                                                                     112-09 150 90 96                                                                250 93 93                                                                      350 95 95                                                                      450 94 98                                                                   ______________________________________                                    

Herbicidal effectiveness overall was very high under the conditions of this study but a tendency can be discerned in compositions 112-01 to 112-04 for performance to improve as butyl stearate concentration was increased from zero to 2%.

Example 113

Aqueous spray compositions were prepared containing various tetraalkylammonium salts of glyphosate and excipient ingredients as shown in Table 113a. Process (iii) was followed for spray compositions 113-02 to 113-04, 113-06 to 113-08, 113-10 to 113-12 and 113-14 to 113-16, using soybean lecithin (45% phospholipid, Avanti). Compositions 113-01, 113-05, 113-09 and 113-13 are simple solutions of the tetraalkylammonium salts of glyphosate in water.

                  TABLE 113a                                                       ______________________________________                                         Spray          % w/w   Glyphosate                                                composition Lecithin salt                                                    ______________________________________                                         113-01                 (Me).sub.4 N                                              113-02 0.10 (Me).sub.4 N                                                       113-03 0.05 (Me).sub.4 N                                                       113-04 0.02 (Me).sub.4 N                                                       113-05  (Et).sub.4 N                                                           113-06 0.10 (Et).sub.4 N                                                       113-07 0.05 (Et).sub.4 N                                                       113-08 0.02 (Et).sub.4 N                                                       113-09  (Pr).sub.4 N                                                           113-10 0.10 (Pr).sub.4 N                                                       113-11 0.05 (Pr).sub.4 N                                                       113-12 0.02 (Pr).sub.4 N                                                       113-13  (Bu).sub.4 N                                                           113-14 0.10 (Bu).sub.4 N                                                       113-15 0.05 (Bu).sub.4 N                                                       113-16 0.02 (Bu).sub.4 N                                                     ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and 20 days after planting ECHCF and evaluation of herbicidal inhibition was done 16 days after application.

Formulations B, C and J were applied as comparative treatments. In addition,

Formulations B and C were tank-mixed with a pre-dispersed lecithin composition prepared from soybean lecithin (45% phospholid, Avanti). Results, averaged for all replicates of each treatment, are shown in Table 113b.

                  TABLE 113b                                                       ______________________________________                                                    Glyphosate                                                            rate % Inhibition                                                            Spray composition                                                                           g a.e./ha   ABUTH    ECUCF                                        ______________________________________                                         Formulation B                                                                               200         23       34                                              400 43 38                                                                      600 69 54                                                                      800 75 41                                                                     Formulation B + 200  7 15                                                      lecithin 0.1% w/v 400 31 36                                                     600 58 37                                                                     Formulation B + 200 10 17                                                      lecithin 0.05% w/v 400 34 40                                                    600 61 47                                                                     Formulation B + 200 11 17                                                      lecithin 0.025% w/v 400 27 39                                                   600 63 39                                                                     Formulation C 200 38 62                                                         400 90 91                                                                      600 96 100                                                                     800 100  99                                                                   Formulation C + 200 36 55                                                      lecithin 0.1% w/v 400 81 93                                                     600 100  95                                                                   Formulation C + 200 35 53                                                      lecithin 0.05% w/v 400 79 90                                                    600 91 99                                                                     Formulation C + 200 32 55                                                      lecithin 0.025% w/v 400 77 88                                                   600 96 100                                                                    Formulation J 200 40 34                                                         400 83 78                                                                      600 87 96                                                                      800 100  95                                                                   113-01 200 27 34                                                                400 74 52                                                                      600 84 46                                                                     113-02 200 39 37                                                                400 73 64                                                                      600 89 68                                                                     113-03 200 24 35                                                                400 73 59                                                                      600 88 75                                                                     113-04 200 29 43                                                                400 71 59                                                                      600 82 90                                                                     113-05 200 51 43                                                                400 79 48                                                                      600 98 49                                                                     113-06 200 58 47                                                                400 84 81                                                                      600 86 97                                                                     113-07 200 69 41                                                                400 83 84                                                                      600 90 94                                                                     113-08 200 55 48                                                                400 79 79                                                                      600 93 92                                                                     113-09 200 73 60                                                                400 96 58                                                                      600 98 73                                                                     113-10 200 69 75                                                                400 94 94                                                                      600 99 91                                                                     113-11 200 72 62                                                                400 94 98                                                                      600 100  99                                                                   113-12 200 76 65                                                                400 97 79                                                                      600 100  100                                                                  113-13 200 85 64                                                                400 97 58                                                                      600 99 65                                                                     113-14 200 83 87                                                                400 99 84                                                                      600 99 98                                                                     113-15 200 87 66                                                                400 94 96                                                                      600 100  100                                                                  113-16 200 91 87                                                                400 97 91                                                                      600 100  94                                                                 ______________________________________                                    

Addition of lecithin to composition B (glyphosate IPA salt) did not provide significant enhancement of herbicidal effectiveness. However, when lecithin was added to tetraalkylammonium salts of glyphosate, significant improvements were obtained. In some cases adding a very low amount of lecithin (0.02%) gave better results than adding a larger amount (0.1%). Outstanding effectiveness, for example, was obtained with composition 113-16, containing the tetrabutylammonium salt of glyphosate and 0.02% lecithin.

Example 114

Aqueous concentrate compositions were prepared containing glyphosate IPA salt and excipient ingredients as shown in Table 114a. Process (v) was followed for all concentrate compositions, using soybean lecithin (45% phospholipid, Avanti).

                  TABLE 114a                                                       ______________________________________                                         Concentrate                                                                              Glyphosate   % w/w                                                   composition                                                                              g a.e./l     Lecithin                                                                               Benzalkonium Cl                                 ______________________________________                                         114-01    363          8.1      5.4                                              114-02 363 8.1  4.1                                                            114-03 363 8.1  3.0                                                            114-04 363 8.1  2.1                                                            114-05 372 8.3  2.5                                                            114-06 363 6.8  4.0                                                            114-07 362 6.8  2.9                                                            114-08 355 3.5 10.0                                                            114-09 354 3.0 13.3                                                            114-10 352 2.5 16.7                                                            114-11 352 2.0 20.0                                                            114-12 295 5.0 10.0                                                            114-13 295 4.5 13.3                                                            114-14 294 4.0 16.7                                                            114-15 294 3.5 20.0                                                            114-16 292 3.0 23.3                                                          ______________________________________                                    

Velvetleaf (Abutilon theophrasti, ABUTH) and Japanese millet (Echinochloa crus-galli, ECHCF) plants were grown and treated by the standard procedures given above. Applications of spray compositions were made 18 days after planting ABUTH and ECHCF, and evaluation of herbicidal inhibition was done 18 days after application.

Formulations B and J were applied as comparative treatments. Results, averaged for all replicates of each treatment, are shown in Table 114b.

                  TABLE 114b                                                       ______________________________________                                                    Glyphosate                                                            Concentrate rate % Inhibition                                                composition                                                                               g a.e./ha     ABUTH    ECHCF                                        ______________________________________                                         Formulation B                                                                             150           52       27                                              250 72 40                                                                      350 87 60                                                                      450 88 77                                                                     Formulation J 150 82 90                                                         250 92 99                                                                      350 99 99                                                                      450 100  100                                                                  114-01 150 78 97                                                                250 87 99                                                                      350 98 99                                                                      450 99 100                                                                    114-02 150 68 83                                                                250 73 99                                                                      350 96 99                                                                      450 98 99                                                                     114-03 150 65 53                                                                250 77 92                                                                      350 93 99                                                                      450 98 100                                                                    114-04 150 62 76                                                                250 83 88                                                                      350 96 98                                                                      450 95 99                                                                     114-05 150 68 57                                                                250 90 88                                                                      350 95 98                                                                      450 98 99                                                                     114-06 150 72 57                                                                250 83 98                                                                      350 93 98                                                                      450 98 100                                                                    114-07 150 77 69                                                                250 85 85                                                                      350 97 98                                                                      450 98 99                                                                     114-08 150 80 85                                                                250 93 99                                                                      350 99 100                                                                     450 100  100                                                                  114-09 150 88 88                                                                250 95 99                                                                      350 100  99                                                                    450 100  100                                                                  114-10 150 99 97                                                                250 97 100                                                                     350 100  100                                                                   450 99 99                                                                     114-11 150 98 92                                                                250 98 97                                                                      350 99 99                                                                      450 100  100                                                                  114-12 150 83 92                                                                250 95 99                                                                      350 98 99                                                                      450 99 99                                                                     114-13 150 91 95                                                                250 94 97                                                                      350 99 100                                                                     450 99 100                                                                    114-14 150 93 96                                                                250 90 97                                                                      350 98 99                                                                      450 99 98                                                                     114-15 150 90 97                                                                250 99 97                                                                      350 100  100                                                                   450 99 99                                                                     114-16 150 92 94                                                                250 98 100                                                                     350 99 100                                                                     450 100  99                                                                 ______________________________________                                    

Overall herbicidal effectiveness in this study was extremely high and enhancements over commercial standard Formulation J are therefore difficult to discern. However, particularly outstanding performance was obtained with compositions 114-10, 114-11 and 114-13 to 114-16 containing lecithin and benzalkonium chloride.

The preceding description of specific embodiments of the present invention is not intended to be a complete list of every possible embodiment of the invention. Persons skilled in this field will recognize that modifications can be made to the specific embodiments described here that would be within the scope of the present invention. 

What is claimed is:
 1. A method of applying an exogenous chemical to a plant, comprising the steps of(a) contacting foliage of the plant with a biologically effective amount of the exogenous chemical, and (b) contacting the same foliage with an aqueous composition that comprises a first excipient substance that is amphiphilic and a second excipient substance selected such that said aqueous composition forms anisotropic aggregates in or on a wax layer, said aqueous composition not forming said anisotropic aggregates in or on a wax layer if said second excipient substance is not present, wherein the weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100; and wherein step (b) occurs simultaneously with or within about 96 hours before or after step (a).
 2. The method of claim 1, wherein the first excipient substance comprises a liposome-forming compound having a hydrophobic moiety comprising two saturated or unsaturated hydrocarbyl groups R¹ and R² each having about 7 to about 21 carbon atoms, said liposome-forming compound having, at a pH of 4, a formula selected from the group consisting of:

    N.sup.+ (CH.sub.2 R.sup.1)(CH.sub.2 R.sup.2)(R.sup.3)(R.sup.4)Z.sup.-(a)

wherein R³ and R⁴ are independently hydrogen, C₁₋₄ alkyl or C₁₋₄ hydroxyalkyl and Z⁻ is a suitable anion;

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH(OCH.sub.2 R.sup.1)CH.sub.2 (OCH.sub.2 R.sup.2)Z.sup.-                                (b)

wherein R⁵, R⁶ and R⁷ are independently hydrogen, C₁₋₄ alkyl or C₁₋₄ hydroxyalkyl and Z⁻ is a suitable anion;

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH(OCOR.sup.1)CH.sub.2 (OCOR.sup.2)Z.sup.-                                       (c)

wherein R⁵, R⁶, R⁷ and Z⁻ are as defined above; and

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH.sub.2 --PO.sub.4.sup.- --CH.sub.2 CH(OCOR.sup.1)CH.sub.2 (OCOR.sup.2)            (d)

wherein R⁵, R⁶ and R⁷ are as defined above.
 3. The method of claim 2, wherein Z⁻ is selected from the group consisting of hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.
 4. The method of claim 3, wherein R¹ and R² are independently saturated straight-chain alkyl groups each having about 7 to about 21 carbon atoms.
 5. The method of claim 2, wherein the first excipient substance is a phospholipid selected from the group consisting of di-C₈₋₂₂ -alkanoylphosphatidylcholines and di-C₈₋₂₂ -alkanoylphosphatidylethanolamines.
 6. The method of claim 5, wherein the first excipient substance is a dipalmitoyl or distearoyl ester of phosphatidylcholine or a mixture thereof.
 7. The method of claim 1, wherein the second excipient substance has one hydrophobic moiety that is a hydrocarbyl or haloalkyl group having about 6 to about 22 carbon atoms, or a plurality of hydrophobic moieties each of which is a hydrocarbyl or haloalkyl group having more than 2 carbon atoms, said plurality of hydrophobic moieties having a total of about 12 to about 40 carbon atoms.
 8. The method of claim 7, wherein said first excipient substance is a liposome-forming substance and said second excipient substance is a quaternary ammonium compound or mixture of such compounds.
 9. The method of claim 8, wherein said quaternary ammonium compound has the formula

    R.sup.8 --W.sub.a --X--Y.sub.b --(CH.sub.2).sub.n --N.sup.+ (R.sup.9)(R.sup.10)(R.sup.11)T.sup.-

wherein R⁸ represents said hydrophobic moiety and is a hydrocarbyl or haloalkyl group having from about 6 to about 22 carbon atoms, W and Y are independently O or NH, a and b are independently 0 or 1 but at least one of a and b is 1, X is CO, SO or SO₂, n is 2 to 4, R⁹, R¹⁰ and R¹¹ are independently C₁₋₄ alkyl, and T is a suitable anion.
 10. The method of claim 9, where R⁸ is hydrocarbyl and has about 12 to about 18 carbon atoms.
 11. The method of claim 9, where R⁸ is fluorinated.
 12. The method of claim 9, where R⁸ is perfluorinated.
 13. The method of claim 12, where R⁸ has about 6 to about 12 carbon atoms.
 14. The method of claim 9, where T is selected from the group consisting of hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.
 15. The method of claim 9, where R⁸ is saturated perfluoroalkyl having about 6 to about 12 carbon atoms, X is CO or SO₂, Y is NH, a is 0, b is 1, R⁹, R¹⁰ and R¹¹ are methyl, and T is selected from the group consisting of hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.
 16. The method of claim 15, where X is SO₂, n is 3 and T is chloride, bromide or iodide.
 17. The method of claim 8 wherein the second excipient substance is 3-(((heptadecafluorooctyl)sulfonyl)amino)-N,N,N-trimethyl-1-propaminium iodide or chloride.
 18. The method of claim 7, wherein said first excipient substance is a liposome-forming substance and said second excipient substance is a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15

wherein R¹⁴ represents said hydrophobic moiety, R¹⁵ is a C₁₋₆ alkyl group and A is O or NH.
 19. The method of claim 7, wherein said first excipient substance is a liposome-forming substance and said second excipient substance is a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15

wherein R¹⁴ is a hydrocarbyl group having about 5 to about 21 carbon atoms, R¹⁵ is a hydrocarbyl group having 1 to about 14 carbon atoms, the total number of carbon atoms in R¹⁴ and R¹⁵ is about 11 to about 27, and A is O or NH.
 20. The method of claim 19 wherein R¹⁴ has about 11 to about 21 carbon atoms, R¹⁵ has 1 to about 6 carbon atoms and A is O.
 21. The method of claim 20 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ fatty acid.
 22. The method of claim 19 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ saturated fatty acid.
 23. The method of claim 19 wherein said second excipient substance is a propyl, isopropyl or butyl ester of a C₁₂₋₁₈ fatty acid.
 24. The method of claim 19 wherein said second excipient substance is butyl stearate.
 25. The method of claim 1, wherein said first excipient substance is an alkylether surfactant or mixture of such surfactants having the formula

    R.sup.12 O--(CH.sub.2 CH.sub.2 O).sub.n (CH(CH.sub.3)CH.sub.2 O).sub.m --R.sup.13

wherein R¹² is an alkyl or alkenyl group having about 16 to about 22 carbon atoms, n is an average number of about 10 to about 100, m is an average number of 0 to about 5 and R¹³ is hydrogen or C₁₋₄ alkyl.
 26. The method of claim 25, wherein m is 0 and R¹³ is hydrogen.
 27. The method of claim 25, wherein n is from about 20 to about
 40. 28. The method of claim 26, wherein R¹² is a saturated straight-chain alkyl group.
 29. The method of claim 28, wherein the alkylether surfactant is a cetyl or stearyl ether or mixture thereof.
 30. The method of claim 25, wherein the second excipient substance comprises a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15

wherein R¹⁴ is a hydrocarbyl having about 5 to about 21 carbon atoms, R¹⁵ is a hydrocarbyl group having 1 to about 14 carbon atoms, the total number of carbon atoms in R¹⁴ and R¹⁵ is about 11 to about 27, and A is O or NH.
 31. The method of claim 30 wherein R¹⁴ has about 11 to about 21 carbon atoms, R¹⁵ has 1 to about 6 carbon atoms and A is O.
 32. The method of claim 31 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ fatty acid.
 33. The method of claim 31 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ saturated fatty acid.
 34. The method of claim 31 wherein said second excipient substance is a propyl, isopropyl or butyl ester of a C₁₂₋₁₈ fatty acid.
 35. The method of claim 31 wherein said second excipient substance is butyl stearate.
 36. The method of claim 30, where the aqueous composition is an emulsion comprising an oil phase that comprises said second excipient substance.
 37. The method of claim 36, where the emulsion is a water-in-oil-in-water multiple emulsion.
 38. The method of claim 36, wherein the emulsion is an oil-in-water emulsion.
 39. The method of claim 1, where the aqueous composition comprises supramolecular aggregates of the first excipient substance which have an average diameter of at least 20 nm.
 40. The method of claim 1, where the aqueous composition comprises supramolecular aggregates of the first excipient substance which have an average diameter of at least 30 nm.
 41. The method of claim 1, wherein the aqueous composition on an epicuticular wax layer on a plant surface forms or enlarges hydrophilic channels through the epicuticular wax layer, the hydrophilic channels being capable of transporting the exogenous chemical into the plant more rapidly or more completely than an epicuticular wax layer lacking such formation or enlargement of hydrophilic channels.
 42. The method of claim 1, wherein the composition forms an aqueous microdomain in or on an epicuticular wax layer on a plant surface, said first excipient substance in the aqueous microdomain being present as bilayers or multilamellar structures.
 43. The method of claim 1, wherein step (b) occurs simultaneously with step (a).
 44. The method of claim 43, wherein the exogenous chemical is contained within said aqueous composition.
 45. The method of claim 1, where the first excipient substance has a critical packing parameter greater than 1/3.
 46. The method of claim 1, wherein the first excipient substance forms aggregates in aqueous solution or dispersion the majority of which are not simple micelles.
 47. The method of claim 1 wherein the exogenous chemical is a foliar-applied exogenous chemical.
 48. The method of claim 47 wherein the exogenous chemical is a pesticide, gametocide or plant growth regulator.
 49. The method of claim 48 wherein the exogenous chemical is a herbicide, nematicide or plant growth regulator.
 50. The method of claim 49 wherein the exogenous chemical is a herbicide.
 51. The method of claim 50 wherein the herbicide is selected from the group consisting of acetanilides, bipyridyls, cyclohexenones, dinitroanilines, diphenylethers, fatty acids, hydroxybenzonitriles, imidazolinones, phenoxies, phenoxypropionates, substituted ureas, sulfonylureas, thiocarbamates and triazines.
 52. The method of claim 50 wherein the herbicide is selected from the group consisting of acetochlor, alachlor, metolachlor, aminotriazole, asulam, bentazon, bialaphos, diquat, paraquat, bromacil, clethodim, sethoxydim, dicamba, diflufenican, pendimethalin, acifluorfen, fomesafen, oxyfluorfen, C₉₋₁₀ fatty acids, fosamine, flupoxam, glufosinate, glyphosate, bromoxynil, imazaquin, imazethapyr, isoxaben, norflurazon, 2,4-D, diclofop, fluazifop, quizalofop, picloram, propanil, fluometuron, isoproturon, chlorimuron, chlorsulfuron, halosulfuron, metsulfuron, primisulfuron, sulfometuron, sulfosulfuron, triallate, atrazine, metribuzin, triclopyr and herbicidal derivatives thereof.
 53. The method of claim 52 wherein the herbicide is glyphosate or a herbicidal derivative thereof.
 54. The method of claim 53 wherein the herbicide is glyphosate in its acid form.
 55. The method of claim 49 wherein the exogenous chemical is water-soluble.
 56. The method of claim 55 wherein the exogenous chemical is a salt having an anion portion and a cation portion.
 57. The method of claim 56 wherein at least one of said anion and cation portions is biologically active and has a molecular weight of less than about
 300. 58. The method of claim 57 wherein the exogenous chemical is paraquat or diquat.
 59. The method of claim 57 wherein the exogenous chemical exhibits systemic biological activity in the plant.
 60. The method of claim 59 wherein the exogenous chemical has one or more functional groups selected from the group consisting of amine, amide, carboxylate, phosphonate and phosphinate groups.
 61. The method of claim 60 wherein the exogenous chemical is a salt of 3,4,4-trifluoro-3-butenoic acid or of N-(3,4,4-trifluoro-1-oxo-3-butenyl)glycine that exhibits nematicidal activity.
 62. The method of claim 60 wherein the exogenous chemical is a herbicidal or plant growth regulating compound having at least one of each of amine, carboxylate and either phosphonate or phosphinate functional groups.
 63. The method of claim 62 wherein the herbicidal or plant growth regulating compound is a salt of glufosinate.
 64. The method of claim 63 wherein the salt of glufosinate is the ammonium salt.
 65. The method of claim 62 wherein the herbicidal or plant growth regulating compound is a salt of N-phosphonomethylglycine.
 66. The method of claim 65 wherein the salt of N-phosphonomethylglycine is selected from the group consisting of sodium, potassium, ammonium, mono-, di-, tri- and tetra-C₁₋₄ -alkylammonium, mono-, di- and tri-C₁₋₄ -alkanolammonium, mono-, di- and tri-C₁₋₄ -alkylsulfonium and sulfoxonium salts.
 67. The method of claim 66 wherein the salt of N-phosphonomethylglycine is the ammonium, monoisopropylammonium or trimethylsulfonium salt.
 68. A plant treatment composition comprising(a) an exogenous chemical, (b) a first excipient substance that is amphiphilic, and (c) a second excipient substance selected such that in presence of water said composition forms anisotropic aggregates in or on a wax layer, said composition not forming said anisotropic aggregates in or on a wax layer in presence of water if said second excipient substance is not present; wherein the weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100.
 69. The composition of claim 68, wherein the composition is a shelf-stable concentrate composition comprising the exogenous chemical substance in an amount of about 15 to about 90 percent by weight.
 70. The composition of claim 69, wherein the composition is a solid composition comprising the exogenous chemical substance in an amount of about 30 to about 90 percent by weight.
 71. The composition of claim 70, wherein the composition is a water-soluble or water-dispersible granular formulation.
 72. The composition of claim 69, further comprising a liquid diluent, and wherein the composition comprises the exogenous chemical substance in an amount of about 15 to about 60 percent by weight.
 73. The composition of claim 72 wherein the exogenous chemical substance is water-soluble and is present in an aqueous phase of the composition in an amount of about 15 to about 45 percent by weight of the composition.
 74. The composition of claim 73, wherein the composition is an aqueous solution concentrate.
 75. The composition of claim 73, wherein the composition is an emulsion having an oil phase.
 76. The composition of claim 75, wherein the composition is an oil-in-water emulsion.
 77. The composition of claim 75, wherein the composition is a water-in-oil emulsion.
 78. The composition of claim 75, wherein the composition is a water-in-oil-in-water multiple emulsion.
 79. The composition of claim 73, further comprising a solid inorganic particulate colloidal material.
 80. The composition of claim 68, further comprising water in an amount effective to make the composition a dilute aqueous composition ready for application to foliage of a plant.
 81. The composition of claim 80, where the composition comprises supramolecular aggregates of the first excipient substance which have an average diameter of at least 20 nm.
 82. The composition of claim 80, where the composition comprises supramolecular aggregates of the first excipient substance which have an average diameter of at least 30 nm.
 83. The composition of claim 68, wherein the composition in the presence of water on an epicuticular wax layer on a plant surface forms or enlarges hydrophilic channels through the epicuticular wax layer, the hydrophilic channels being capable of transporting the exogenous chemical into the plant more rapidly or more completely than an epicuticular wax layer lacking such formation or enlargement of hydrophilic channels.
 84. The composition of claim 68, wherein the composition in the presence of water in or on an epicuticular wax layer on a plant surface forms an aqueous microdomain, said first excipient substance in the aqueous microdomain being present as bilayers or multilamellar structures.
 85. The composition of claim 68, wherein the first excipient substance comprises a liposome-forming compound having a hydrophobic moiety comprising two saturated or unsaturated hydrocarbyl groups R¹ and R² each having about 7 to about 21 carbon atoms, said liposome-forming compound having, at a pH of 4, a formula selected from the group consisting of:

    N.sup.+ (CH.sub.2 R.sup.1)(CH.sub.2 R.sup.2)(R.sup.3)(R.sup.4)Z.sup.-(a)

wherein R³ and R⁴ are independently hydrogen, C₁₋₄ alkyl or C₁₋₄ hydroxyalkyl and Z⁻ is a suitable anion;

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH(OCH.sub.2 R.sup.1)CH.sub.2 (OCH.sub.2 R.sup.2)Z.sup.-                                (b)

wherein R⁵, R⁶ and R⁷ are independently hydrogen, C₁₋₄ alkyl or C₁₋₄ hydroxyalkyl and Z⁻ is a suitable anion;

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH(OCOR.sup.1)CH.sub.2 (OCOR.sup.2)Z.sup.-                                       (c)

wherein R⁵, R⁶, R⁷ and Z⁻ are as defined above; and

    N.sup.+ (R.sup.5)(R.sup.6)(R.sup.7)CH.sub.2 CH.sub.2 --PO.sub.4.sup.- --CH.sub.2 CH(OCOR.sup.1)CH.sub.2 (OCOR.sup.2)            (d)

wherein R⁵, R⁶ and R⁷ are as defined above.
 86. The composition of claim 85, wherein Z⁻ is selected from the group consisting of hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.
 87. The composition of claim 86, wherein R¹ and R² are independently saturated straight-chain alkyl groups each having about 7 to about 21 carbon atoms.
 88. The composition of claim 85, wherein the first excipient substance is a phospholipid selected from the group consisting of di-C₈₋₂₂ -alkanoylphosphatidylcholines and di-C₈₋₂₂ -alkanoylphosphatidylethanolamines.
 89. The composition of claim 88, wherein the first excipient substance is a dipalmitoyl or distearoyl ester of phosphatidylcholine or a mixture thereof.
 90. The composition of claim 68, wherein the second excipient substance has one hydrophobic moiety that is a hydrocarbyl or haloalkyl group having about 6 to about 22 carbon atoms, or a plurality of hydrophobic moieties each of which is a hydrocarbyl or haloalkyl group having more than 2 carbon atoms, said plurality of hydrophobic moieties having a total of about 12 to about 40 carbon atoms.
 91. The composition of claim 90, wherein said first excipient substance is a liposome-forming substance and said second excipient substance is a quaternary ammonium compound or mixture of such compounds.
 92. The composition of claim 91, wherein said quaternary ammonium compound has the formula

    R.sup.8 --W.sub.a --X--Y.sub.b --(CH.sub.2).sub.n --N.sup.+ (R.sup.9)(R.sup.10)(R.sup.11)T.sup.-

wherein R⁸ represents said hydrophobic moiety and is a hydrocarbyl or haloalkyl group having from about 6 to about 22 carbon atoms, W and Y are independently O or NH, a and b are independently 0 or 1 but at least one of a and b is 1, X is CO, SO or SO₂, n is 2 to 4, R⁹, R¹⁰ and R¹¹ are independently C₁₋₄ alkyl, and T is a suitable anion.
 93. The composition of claim 92, where R⁸ is hydrocarbyl and has about 12 to about 18 carbon atoms.
 94. The composition of claim 92, where R⁸ is fluorinated.
 95. The composition of claim 92, where R⁸ is perfluorinated.
 96. The composition of claim 95, where R⁸ has about 6 to about 12 carbon atoms.
 97. The composition of claim 92, where T is selected from the group consisting of hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.
 98. The composition of claim 92, where R⁸ is saturated perfluoroalkyl having about 6 to about 12 carbon atoms, X is CO or SO₂, Y is NH, a is 0, b is 1, R⁹,R¹⁰ and R¹¹ are methyl, and T is selected from the group consisting of hydroxide, chloride, bromide, iodide, sulfate, phosphate and acetate.
 99. The composition of claim 98, where X is SO₂, n is 3 and T is chloride, bromide or iodide.
 100. The composition of claim 91 wherein the second excipient substance is 3-(((heptadecafluorooctyl)sulfonyl)amino)-N,N,N-trimethyl-1-propaminium iodide or chloride.
 101. The composition of claim 90, wherein said first excipient substance is a liposome-forming substance and said second excipient substance is a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15

wherein R¹⁴ represents said hydrophobic moiety, R¹⁵ is a C₁₋₆ alkyl group and A is O or NH.
 102. The composition of claim 90, wherein said first excipient substance is a liposome-forming substance and said second excipient substance is a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15

wherein R¹⁴ is a hydrocarbyl group having about 5 to about 21 carbon atoms, R¹⁵ is a hydrocarbyl group having 1 to about 14 carbon atoms, the total number of carbon atoms in R¹⁴ and R¹⁵ is about 11 to about 27, and A is O or NH.
 103. The composition of claim 102 wherein R¹⁴ has about 11 to about 21 carbon atoms, R¹⁵ has 1 to about 6 carbon atoms and A is O.
 104. The composition of claim 103 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ fatty acid.
 105. The composition of claim 102 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ saturated fatty acid.
 106. The composition of claim 102 wherein said second excipient substance is a propyl, isopropyl or butyl ester of a C₁₂₋₁₈ fatty acid.
 107. The composition of claim 102 wherein said second excipient substance is butyl stearate.
 108. The composition of claim 68, wherein said first excipient substance is an alkylether surfactant or mixture of such surfactants having the formula

    R.sup.12 O--(CH.sub.2 CH.sub.2 O).sub.n (CH(CH.sub.3)CH.sub.2 O).sub.m --R.sup.13

wherein R¹² is an alkyl or alkenyl group having about 16 to about 22 carbon atoms, n is an average number of about 10 to about 100, m is an average number of 0 to about 5 and R¹³ is hydrogen or C₁₋₄ alkyl.
 109. The composition of claim 108, wherein m is 0 and R¹³ is hydrogen.
 110. The composition of claim 108, wherein n is from about 20 to about
 40. 111. The composition of claim 109, wherein R¹² is a saturated straight-chain alkyl group.
 112. The composition of claim 111, wherein the alkylether surfactant is a cetyl or stearyl ether or mixture thereof.
 113. The composition of claim 108, wherein the second excipient substance comprises a compound or mixture of compounds of formula

    R.sup.14 --CO--A--R.sup.15

wherein R¹⁴ is a hydrocarbyl having about 5 to about 21 carbon atoms, R¹⁵ is a hydrocarbyl group having 1 to about 14 carbon atoms, the total number of carbon atoms in R¹⁴ and R¹⁵ is about 11 to about 27, and A is O or NH.
 114. The composition of claim 113 wherein R¹⁴ has about 11 to about 21 carbon atoms, R¹⁵ has 1 to about 6 carbon atoms and A is O.
 115. The composition of claim 114 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ fatty acid.
 116. The composition of claim 114 wherein said second excipient substance is a C₁₋₄ alkyl ester of a C₁₂₋₁₈ saturated fatty acid.
 117. The composition of claim 114 wherein said second excipient substance is a propyl, isopropyl or butyl ester of a C₁₂₋₁₈ fatty acid.
 118. The composition of claim 114 wherein said second excipient substance is butyl stearate.
 119. The composition of claim 68, where the first excipient substance has a critical packing parameter greater than 1/3.
 120. The composition of claim 68, wherein the first excipient substance forms aggregates in aqueous solution or dispersion the majority of which are not simple micelles.
 121. The composition of claim 68 wherein the exogenous chemical is a foliar-applied exogenous chemical.
 122. The composition of claim 121 wherein the exogenous chemical is a pesticide, gametocide or plant growth regulator.
 123. The composition of claim 122 wherein the exogenous chemical is a herbicide, nematicide or plant growth regulator.
 124. The composition of claim 123 wherein the exogenous chemical is a herbicide.
 125. The composition of claim 124 wherein the herbicide is selected from the group consisting of acetanilides, bipyridyls, cyclohexenones, dinitroanilines, diphenylethers, fatty acids, hydroxybenzonitriles, imidazolinones, phenoxies, phenoxypropionates, substituted ureas, sulfonylureas, thiocarbamates and triazines.
 126. The composition of claim 124 wherein the herbicide is selected from the group consisting of acetochlor, alachlor, metolachlor, aminotriazole, asulam, bentazon, bialaphos, diquat, paraquat, bromacil, clethodim, sethoxydim, dicamba, diflufenican, pendimethalin, acifluorfen, C₉₋₁₀ fatty acids, fomesafen, oxyfluorfen, fosamine, flupoxam, glufosinate, glyphosate, bromoxynil, imazaquin, imazethapyr, isoxaben, norflurazon, 2,4-D, diclofop, fluazifop, quizalofop, picloram, propanil, fluometuron, isoproturon, chlorimuron, chlorsulfuron, halosulfuron, metsulfuron, primisulfuron, sulfometuron, sulfosulfuron, triallate, atrazine, metribuzin, triclopyr and herbicidal derivatives thereof.
 127. The composition of claim 126 wherein the herbicide is glyphosate or a herbicidal derivative thereof.
 128. The composition of claim 127 wherein the herbicide is glyphosate in its acid form.
 129. The composition of claim 123 wherein the exogenous chemical is water-soluble.
 130. The composition of claim 129 wherein the exogenous chemical is a salt having an anion portion and a cation portion.
 131. The composition of claim 130 wherein at least one of said anion and cation portions is biologically active and has a molecular weight of less than about
 300. 132. The composition of claim 131 wherein the exogenous chemical is paraquat or diquat.
 133. The composition of claim 131 wherein the exogenous chemical exhibits systemic biological activity in the plant.
 134. The composition of claim 133 wherein the exogenous chemical has one or more functional groups selected from the group consisting of amine, amide, carboxylate, phosphonate and phosphinate groups.
 135. The composition of claim 134 wherein the exogenous chemical is a salt of 3,4,4-trifluoro-3-butenoic acid or of N-(3,4,4-trifluoro-1-oxo-3-butenyl)glycine that exhibits nematicidal activity.
 136. The composition of claim 134 wherein the exogenous chemical is a herbicidal or plant growth regulating compound having at least one of each of amine, carboxylate and either phosphonate or phosphinate functional groups.
 137. The composition of claim 136 wherein the herbicidal or plant growth regulating compound is a salt of glufosinate.
 138. The composition of claim 137 wherein the salt of glufosinate is the ammonium salt.
 139. The composition of claim 136 wherein the herbicidal or plant growth regulating compound is a salt of N-phosphonomethylglycine.
 140. The composition of claim 139 wherein the salt of N-phosphonomethylglycine is selected from the group consisting of sodium, potassium, ammonium, mono-, di-, tri- and tetra-C₁₋₄ -alkylammonium, mono-, di- and tri-C₁₋₄ -alkanolammonium, mono-, di- and tri-C₁₋₄ -alkylsulfonium and sulfoxonium salts.
 141. The composition of claim 140 wherein the salt of N-phosphonomethylglycine is the ammonium, monoisopropylammonium or trimethylsulfonium salt.
 142. The composition of claim 113, where the aqueous composition is an emulsion comprising an oil phase that comprises said second excipient substance.
 143. The composition of claim 142, where the emulsion is a water-in-oil-in-water multiple emulsion.
 144. The composition of claim 142, wherein the emulsion is an oil-in-water emulsion.
 145. A plant treatment method, comprising the step of contacting foliage of a plant with a biologically effective amount of a composition according to any of claims 68, 80-99, or 101-144.
 146. A method for enhancing the yield of a field crop comprising the steps of:(a) planting a crop in a field; (b) substantially freeing the field of one or more weed species that would diminish the yield of the crop by applying to the weed species a herbicidally effective amount of a composition that comprises (i) a foliar herbicide, (ii) an aqueous diluent, (iii) a first excipient substance that is amphiphilic, and (iv) a second excipient substance selected such that in presence of water said composition forms anisotropic aggregates in or on a wax layer, said composition not forming said anisotropic aggregates in or on a wax layer in presence of water if said second excipient substance is not present; wherein the weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100; (c) allowing the crop to mature; and (d) harvesting the crop.
 147. A method for enhancing the yield of a field crop comprising the steps of:(a) substantially freeing a field of one or more weed species that would diminish the yield of the crop by applying to the weed species a herbicidally effective amount of a composition that comprises (i) a foliar herbicide, (ii) an aqueous diluent, (iii) a first excipient substance that is amphiphilic, and (iv) a second excipient substance selected such that in presence of water said composition forms anisotropic aggregates in or on a wax layer, said composition not forming said anisotropic aggregates in or on a wax layer in presence of water if said second excipient substance is not present; wherein the weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100; (b) planting the crop in the field; (c) allowing the crop to mature; and (d) harvesting the crop.
 148. A plant treatment, comprising contacting foliage of a plant with a composition comprising(a) water, (b) a biologically effective amount of an exogenous chemical, (c) a first excipient substance that is amphiphilic, and (d) a second excipient substance selected such that in presence of water said composition forms anisotropic aggregates in or on a wax layer, said composition not forming said anisotropic aggregates in or on a wax layer in presence of water if said second excipient substance is not present;wherein the weight/weight ratio of said first excipient substance to the exogenous chemical is between about 1:3 and about 1:100; and wherein the biological effectiveness of the composition is greater than that of otherwise similar compositions that do not form such anisotropic aggregates. 